#------------------------------------------------------------------------------ #$Date: 2021-03-28 04:49:57 +0300 (Sun, 28 Mar 2021) $ #$Revision: 263395 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/13/1561311.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_1561311 loop_ _publ_author_name 'H\"afliger, Joel' 'Livingstone, Keith' 'Daniliuc, Constantin' 'Gilmour, Ryan' _publ_section_title ; Difluorination of \a-(Bromomethyl)styrenes via I(I)/I(III) Catalysis: Facile Access to Electrophilic Linchpins for Drug Discovery ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC01132D _journal_year 2021 _chemical_formula_sum 'C17 H12 Br F2 N O2' _chemical_formula_weight 380.19 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method 'APEX3 v2019.11-0' _audit_update_record ; 2021-01-13 deposited with the CCDC. 2021-03-26 downloaded from the CCDC. ; _cell_angle_alpha 67.712(5) _cell_angle_beta 85.665(5) _cell_angle_gamma 88.114(6) _cell_formula_units_Z 2 _cell_length_a 4.7731(8) _cell_length_b 11.3543(17) _cell_length_c 14.650(2) _cell_measurement_reflns_used 6241 _cell_measurement_temperature 102.(2) _cell_measurement_theta_max 26.8468 _cell_measurement_theta_min 2.8698 _cell_volume 732.53(19) _computing_cell_refinement 'SAINT V8.40B (Bruker Nano, Inc., 2019)' _computing_data_collection 'Bruker APEX3 v2019.11-0 Photon III' _computing_data_reduction 'SAINT V8.40B (Bruker Nano, Inc., 2019)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 994)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 102.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device 'Bruker D8 Venture Photon III Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method 'phi/omega scans' _diffrn_radiation_monochromator 'MX mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_unetI/netI 0.0391 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 14235 _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_min 2.87 _diffrn_source MoK\a _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'micro focus tube' _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 2.837 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction. Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 380 _exptl_crystal_size_max 0.149 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.043 _refine_diff_density_max 0.613 _refine_diff_density_min -0.485 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 2620 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0333 _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^+0.5703P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.0779 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2325 _reflns_number_total 2620 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc01132d2.cif _cod_data_source_block gil9967 _cod_original_cell_volume 732.5(2) _cod_database_code 1561311 _shelx_res_file ; TITL gil9967.res in P-1 gil9967.res created by SHELXL-2018/3 at 07:52:42 on 11-Dec-2020 CELL 0.71073 4.7731 11.3543 14.6499 67.712 85.665 88.114 ZERR 2.000 0.0008 0.0017 0.0024 0.005 0.005 0.006 LATT 1 SFAC C H Br F N O UNIT 34 24 2 4 2 4 LIST 4 SIZE 0.043 0.085 0.149 TEMP -171.150 ACTA CONF SHEL 999 0.83 OMIT -1 4 1 OMIT 3 0 9 OMIT 1 6 2 L.S. 30 BOND $H FMAP 2 PLAN 10 WGHT 0.038400 0.570300 FVAR 0.60832 BR1 3 -0.276878 0.164132 0.969510 11.00000 0.02430 0.02291 = 0.01763 -0.00933 -0.00035 -0.00478 N1 5 0.446918 0.303325 0.346048 11.00000 0.01491 0.01242 = 0.01591 -0.00671 0.00001 -0.00164 O1 6 0.524186 0.518738 0.314501 11.00000 0.01782 0.01280 = 0.02458 -0.00948 0.00086 -0.00251 O2 6 0.485280 0.106645 0.328793 11.00000 0.02143 0.01445 = 0.02522 -0.01102 0.00166 -0.00480 C1 1 0.235985 0.274125 0.427063 11.00000 0.01303 0.01487 = 0.01874 -0.00961 -0.00127 -0.00106 C2 1 0.209819 0.149151 0.496755 11.00000 0.01703 0.01305 = 0.02078 -0.00761 -0.00041 0.00033 AFIX 43 H2 2 0.329733 0.083735 0.490592 11.00000 -1.20000 AFIX 0 C3 1 0.005607 0.121776 0.575368 11.00000 0.01545 0.01332 = 0.01924 -0.00614 -0.00105 -0.00292 AFIX 43 H3 2 -0.015690 0.036648 0.621565 11.00000 -1.20000 AFIX 0 C4 1 -0.165658 0.215844 0.587246 11.00000 0.01179 0.01765 = 0.01776 -0.00930 -0.00176 -0.00617 C5 1 -0.136957 0.339620 0.517292 11.00000 0.01339 0.01469 = 0.02317 -0.01310 -0.00325 0.00182 AFIX 43 H5 2 -0.254830 0.405115 0.524375 11.00000 -1.20000 AFIX 0 C6 1 0.061933 0.369121 0.436969 11.00000 0.01542 0.01388 = 0.01916 -0.00755 -0.00490 -0.00122 AFIX 43 H6 2 0.077633 0.453745 0.389496 11.00000 -1.20000 AFIX 0 C7 1 -0.377437 0.187751 0.675609 11.00000 0.01245 0.01422 = 0.02183 -0.00927 0.00028 -0.00281 AFIX 23 H7A 2 -0.522126 0.255745 0.659896 11.00000 -1.20000 H7B 2 -0.472483 0.106345 0.688149 11.00000 -1.20000 AFIX 0 C8 1 -0.242095 0.179090 0.768492 11.00000 0.01532 0.01062 = 0.02421 -0.00855 -0.00088 -0.00077 F1 4 -0.072870 0.072419 0.800556 11.00000 0.02210 0.01731 = 0.02610 -0.01053 -0.00426 0.00564 F2 4 -0.060633 0.279673 0.747330 11.00000 0.01620 0.01840 = 0.02240 -0.01006 0.00116 -0.00753 C9 1 -0.455225 0.177370 0.850405 11.00000 0.01543 0.02233 = 0.01881 -0.00847 -0.00041 -0.00323 AFIX 23 H9A 2 -0.583073 0.104310 0.866293 11.00000 -1.20000 H9B 2 -0.569404 0.256298 0.827539 11.00000 -1.20000 AFIX 0 C10 1 0.576811 0.424264 0.298192 11.00000 0.01317 0.01557 = 0.01621 -0.00509 -0.00501 -0.00071 C11 1 0.795165 0.407888 0.224829 11.00000 0.01265 0.01665 = 0.01579 -0.00665 -0.00449 0.00098 C12 1 0.985443 0.495354 0.161020 11.00000 0.01674 0.01826 = 0.01798 -0.00748 -0.00178 -0.00235 AFIX 43 H12 2 0.989826 0.580553 0.157526 11.00000 -1.20000 AFIX 0 C13 1 1.170484 0.452214 0.102085 11.00000 0.01476 0.02586 = 0.02031 -0.00973 0.00003 -0.00272 AFIX 43 H13 2 1.304975 0.509291 0.057416 11.00000 -1.20000 AFIX 0 C14 1 1.162781 0.327715 0.107159 11.00000 0.01458 0.02758 = 0.01853 -0.01088 -0.00111 0.00227 AFIX 43 H14 2 1.291713 0.301354 0.065901 11.00000 -1.20000 AFIX 0 C15 1 0.968624 0.240487 0.171915 11.00000 0.01860 0.01672 = 0.02007 -0.00963 -0.00335 0.00141 AFIX 43 H15 2 0.962230 0.155243 0.175623 11.00000 -1.20000 AFIX 0 C16 1 0.786707 0.283843 0.230197 11.00000 0.01385 0.01711 = 0.01530 -0.00526 -0.00375 -0.00058 C17 1 0.560478 0.215256 0.306050 11.00000 0.01253 0.01613 = 0.01813 -0.00787 -0.00263 -0.00089 HKLF 4 REM gil9967.res in P-1 REM wR2 = 0.077851, GooF = S = 1.06762, Restrained GooF = 1.06762 for all data REM R1 = 0.033262 for 2325 Fo > 4sig(Fo) and 0.039269 for all 2620 data REM 208 parameters refined using 0 restraints END WGHT 0.0378 0.5755 REM Highest difference peak 0.613, deepest hole -0.485, 1-sigma level 0.083 Q1 1 -0.3109 0.1194 1.0393 11.00000 0.05 0.61 Q2 1 -0.2634 0.2021 0.9021 11.00000 0.05 0.60 Q3 1 -0.0948 0.1180 0.9663 11.00000 0.05 0.49 Q4 1 -0.4981 0.1752 0.9589 11.00000 0.05 0.42 Q5 1 0.6873 0.2467 0.2648 11.00000 0.05 0.36 Q6 1 -0.4299 0.2254 0.9848 11.00000 0.05 0.36 Q7 1 -0.3034 0.1797 0.7203 11.00000 0.05 0.32 Q8 1 1.0360 0.4718 0.1121 11.00000 0.05 0.30 Q9 1 0.9274 0.4407 0.2028 11.00000 0.05 0.30 Q10 1 0.3566 0.2752 0.3908 11.00000 0.05 0.30 ; _shelx_res_checksum 74722 _shelx_hkl_file ; -1 0 0 63.49 5.00 -1 0 0 56.79 5.00 1 0 0 57.29 5.00 1 0 0 54.79 4.40 1 0 0 62.69 5.00 -2 0 0 10.00 3.50 -2 0 0 10.40 3.90 -2 0 0 15.50 4.50 2 0 0 9.30 3.30 2 0 0 14.60 4.20 2 0 0 14.70 4.50 -3 0 0 14.80 4.60 -3 0 0 11.60 5.00 3 0 0 24.00 5.40 3 0 0 14.30 5.30 3 0 0 23.00 6.30 -4 0 0 593.24 30.10 -4 0 0 546.15 30.80 4 0 0 537.85 29.60 4 0 0 558.44 28.90 4 0 0 555.54 31.40 -5 0 0 6.60 6.50 5 0 0 9.10 6.70 5 0 0 9.40 8.50 5 0 0 2.80 6.60 -6 0 0 12.50 8.60 6 0 0 20.20 11.00 6 0 0 29.90 10.20 6 0 0 17.30 13.20 6 -1 0 1.50 7.60 6 -1 0 5.40 12.20 6 -1 0 -2.10 7.30 -6 1 0 8.60 7.90 5 -1 0 349.67 23.90 5 -1 0 339.37 23.00 5 -1 0 286.67 23.10 -5 1 0 224.48 24.30 -5 1 0 298.27 21.20 4 -1 0 16.30 5.80 4 -1 0 12.60 7.40 4 -1 0 9.90 6.50 -4 1 0 16.90 6.10 -4 1 0 10.40 5.80 3 -1 0 365.86 20.30 3 -1 0 359.66 21.00 3 -1 0 385.96 19.70 -3 1 0 352.06 20.60 -3 1 0 390.16 20.10 2 -1 0 86.99 8.10 2 -1 0 77.59 6.80 2 -1 0 77.29 7.70 -2 1 0 70.69 7.50 -2 1 0 86.89 7.10 1 -1 0 2606.14 106.19 -1 1 0 2624.74 105.89 -1 1 0 2586.04 106.19 -1 -1 0 1682.63 69.59 -1 -1 0 1714.03 69.59 -1 -1 0 1689.43 70.19 1 1 0 1665.53 69.49 1 1 0 1730.23 70.29 1 1 0 1666.43 69.59 -2 -1 0 220.78 13.40 -2 -1 0 227.58 13.00 2 1 0 203.48 12.20 2 1 0 217.98 13.50 2 1 0 214.28 12.90 -3 -1 0 15.00 5.70 -3 -1 0 13.50 5.00 -3 -1 0 12.40 4.70 3 1 0 11.40 4.50 3 1 0 7.90 5.30 3 1 0 14.80 5.70 -4 -1 0 359.56 21.80 -4 -1 0 317.97 22.20 4 1 0 382.06 23.90 4 1 0 331.17 21.80 4 1 0 353.56 20.80 -5 -1 0 0.10 6.50 -5 -1 0 10.80 7.60 5 1 0 7.10 7.30 5 1 0 5.20 8.30 5 1 0 8.40 6.70 -6 -1 0 74.59 13.50 6 1 0 80.69 13.40 6 1 0 110.99 16.80 6 1 0 80.09 15.00 5 -2 0 63.79 12.60 5 -2 0 82.99 14.30 5 -2 0 87.09 12.10 -5 2 0 70.69 11.90 -5 2 0 73.49 11.90 4 -2 0 311.97 21.00 4 -2 0 285.67 19.90 4 -2 0 293.57 18.40 -4 2 0 313.17 19.10 -4 2 0 298.77 19.90 3 -2 0 40.40 7.40 3 -2 0 40.80 7.20 3 -2 0 42.10 6.20 -3 2 0 38.90 6.40 -3 2 0 45.30 7.20 2 -2 0 777.22 35.10 2 -2 0 767.22 34.30 -2 2 0 812.72 34.50 -2 2 0 774.72 35.10 1 -2 0 1126.69 48.00 1 -2 0 1166.78 47.70 -1 2 0 1096.99 47.90 -1 2 0 1233.48 47.70 0 -2 0 2295.07 92.59 0 2 0 2177.68 92.59 -1 -2 0 1397.86 56.89 -1 -2 0 1358.06 56.19 -1 -2 0 1323.07 56.29 1 2 0 1290.67 56.99 1 2 0 1381.86 56.99 -2 -2 0 183.38 11.90 -2 -2 0 180.38 11.60 -2 -2 0 163.08 11.80 2 2 0 185.58 12.60 2 2 0 169.18 11.70 2 2 0 173.68 10.90 -3 -2 0 171.08 13.50 -3 -2 0 170.78 13.10 -3 -2 0 168.88 12.90 3 2 0 168.08 13.70 3 2 0 179.18 13.10 3 2 0 161.18 11.90 -4 -2 0 39.10 9.50 -4 -2 0 20.20 6.70 -4 -2 0 35.20 8.80 4 2 0 21.80 6.30 4 2 0 34.90 8.90 4 2 0 30.20 9.10 -5 -2 0 119.39 16.50 -5 -2 0 105.29 14.60 5 2 0 125.29 13.70 5 2 0 123.29 17.30 5 2 0 130.19 15.90 5 -3 0 54.99 11.70 5 -3 0 32.50 8.40 5 -3 0 23.80 9.30 -5 3 0 26.40 8.70 -5 3 0 9.70 6.40 4 -3 0 338.07 22.30 4 -3 0 372.56 23.20 4 -3 0 345.47 20.70 -4 3 0 394.46 21.50 -4 3 0 358.56 22.20 3 -3 0 52.79 8.00 3 -3 0 45.30 6.50 -3 3 0 47.60 6.90 -3 3 0 47.40 6.60 2 -3 0 492.45 23.40 -2 3 0 476.25 23.10 -2 3 0 497.05 22.50 1 -3 0 652.43 27.80 1 -3 0 651.93 34.40 0 -3 0 3058.69 125.19 0 -3 0 3154.58 123.29 0 3 0 2842.92 125.29 -1 -3 0 454.85 22.30 -1 -3 0 451.75 21.40 -1 -3 0 460.55 20.80 -1 -3 0 441.36 22.00 1 3 0 457.45 21.20 1 3 0 442.06 21.40 1 3 0 461.95 20.50 1 3 0 444.36 22.80 -2 -3 0 167.88 11.40 -2 -3 0 167.18 11.90 -2 -3 0 159.18 11.70 2 3 0 142.19 13.00 2 3 0 153.78 10.40 2 3 0 164.78 12.10 2 3 0 156.68 11.40 -3 -3 0 274.07 17.50 -3 -3 0 245.18 16.50 3 3 0 252.07 16.50 3 3 0 240.98 15.50 3 3 0 265.17 17.70 -4 -3 0 442.56 25.20 -4 -3 0 393.66 24.50 -4 -3 0 412.26 24.60 -4 -3 0 391.36 25.40 4 3 0 402.76 24.50 4 3 0 405.16 23.50 4 3 0 424.16 26.60 -5 -3 0 28.60 10.10 -5 -3 0 36.70 15.20 -5 -3 0 31.90 9.00 -5 -3 0 42.60 10.60 5 3 0 21.50 8.30 5 3 0 23.20 9.30 5 3 0 39.30 11.50 5 -4 0 193.08 19.70 5 -4 0 207.58 16.80 5 -4 0 225.38 19.40 -5 4 0 228.48 16.90 -5 4 0 199.98 17.80 4 -4 0 53.59 8.60 -4 4 0 65.49 9.60 -4 4 0 33.10 7.70 3 -4 0 300.37 18.30 3 -4 0 295.77 16.80 -3 4 0 339.17 17.20 2 -4 0 95.39 8.00 -2 4 0 96.09 7.60 -2 4 0 101.69 7.10 1 -4 0 1251.77 59.59 0 -4 0 164.58 13.90 0 -4 0 168.48 8.40 0 -4 0 172.58 8.90 0 4 0 169.68 8.60 -1 -4 0 939.61 42.60 -1 -4 0 946.71 41.40 -1 -4 0 951.40 40.60 -1 -4 0 931.81 41.40 1 4 0 974.90 41.40 1 4 0 825.92 43.40 1 4 0 956.50 40.30 1 4 0 1006.90 41.70 -2 -4 0 1805.32 77.49 -2 -4 0 1848.81 76.59 -2 -4 0 1853.31 76.99 2 4 0 1827.02 76.09 2 4 0 1789.92 77.79 2 4 0 1764.32 76.59 2 4 0 1701.43 77.99 -3 -4 0 178.78 20.70 -3 -4 0 136.69 13.00 3 4 0 151.58 11.80 3 4 0 160.88 13.90 3 4 0 135.89 15.40 3 4 0 154.18 13.00 -4 -4 0 7.00 5.70 -4 -4 0 13.80 6.70 4 4 0 10.00 6.90 4 4 0 12.40 5.90 4 4 0 12.40 7.50 -5 -4 0 15.40 7.10 -5 -4 0 13.40 8.40 -5 -4 0 12.90 8.60 -5 -4 0 9.20 8.00 5 4 0 7.30 8.90 5 4 0 15.40 7.20 5 4 0 16.80 8.80 5 -5 0 4.80 10.20 5 -5 0 3.70 7.10 5 -5 0 8.80 6.30 -5 5 0 10.20 6.30 -5 5 0 5.10 7.20 4 -5 0 11.50 8.20 4 -5 0 14.80 5.70 4 -5 0 7.00 6.70 -4 5 0 15.50 6.10 -4 5 0 15.60 5.40 3 -5 0 237.08 13.90 3 -5 0 238.78 15.30 -3 5 0 237.38 13.80 2 -5 0 1174.68 62.39 1 -5 0 121.39 17.30 0 -5 0 71.19 8.90 0 -5 0 70.19 14.00 0 -5 0 51.89 5.50 0 -5 0 48.90 4.90 0 5 0 50.79 11.00 0 5 0 49.00 4.80 -1 -5 0 769.72 33.70 -1 -5 0 762.12 35.10 -1 -5 0 769.82 34.60 1 5 0 778.32 33.40 1 5 0 785.02 34.80 1 5 0 760.52 34.90 1 5 0 694.13 37.80 -2 -5 0 104.39 10.50 -2 -5 0 84.79 9.40 -2 -5 0 91.49 9.00 2 5 0 78.99 13.90 2 5 0 99.39 10.00 2 5 0 87.79 8.10 2 5 0 85.79 9.70 -3 -5 0 736.43 38.30 -3 -5 0 803.92 38.00 3 5 0 758.22 36.40 3 5 0 794.82 39.40 3 5 0 746.23 40.20 3 5 0 747.93 37.50 -4 -5 0 58.19 12.40 -4 -5 0 52.09 10.10 -4 -5 0 52.29 11.00 -4 -5 0 47.50 10.80 4 5 0 43.50 8.60 4 5 0 47.80 11.30 4 5 0 52.19 10.90 -5 -5 0 19.10 8.70 -5 -5 0 3.60 5.80 -5 -5 0 14.80 9.50 -5 -5 0 3.10 8.30 5 5 0 3.80 7.20 5 5 0 7.60 7.70 5 -6 0 49.90 13.30 5 -6 0 50.29 10.30 5 -6 0 58.59 29.50 5 -6 0 58.69 9.90 -5 6 0 47.10 9.70 4 -6 0 373.36 25.40 4 -6 0 439.46 45.50 4 -6 0 323.77 21.90 -4 6 0 384.76 20.30 3 -6 0 13.10 16.20 3 -6 0 5.20 4.10 3 -6 0 8.80 5.60 -3 6 0 7.40 3.60 -3 6 0 6.00 4.30 2 -6 0 384.06 31.70 1 -6 0 366.96 27.30 0 -6 0 587.54 27.60 0 -6 0 505.95 24.10 0 -6 0 592.24 31.80 0 6 0 522.45 31.80 -1 -6 0 1.00 8.70 -1 -6 0 1.30 5.10 -1 -6 0 -1.40 3.10 -1 -6 0 -0.60 3.40 1 6 0 -2.10 2.30 1 6 0 1.40 8.10 1 6 0 -1.10 3.40 1 6 0 -0.10 4.60 -2 -6 0 682.63 34.00 -2 -6 0 705.03 33.20 -2 -6 0 742.23 34.60 2 6 0 724.33 34.70 2 6 0 679.43 32.30 2 6 0 703.13 33.90 2 6 0 626.84 36.70 -3 -6 0 110.09 13.40 -3 -6 0 78.39 11.90 3 6 0 93.19 12.40 3 6 0 115.19 18.20 3 6 0 80.69 9.30 3 6 0 96.59 12.90 -4 -6 0 8.90 8.00 -4 -6 0 3.30 9.60 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0 -3 -16 142.69 17.90 0 -3 -16 160.08 20.60 0 -3 -16 163.58 29.00 0 3 16 172.98 22.60 0 3 16 157.98 16.60 0 3 16 151.08 22.20 0 3 16 158.68 16.20 -1 -3 -16 13.10 8.10 -1 -3 -16 2.20 10.00 -1 -3 -16 13.50 20.30 -1 -3 -16 5.90 8.00 1 3 16 22.90 8.70 1 3 16 10.10 7.50 1 3 16 26.30 14.90 1 3 16 6.70 13.30 -2 -3 -16 151.98 22.20 -2 -3 -16 201.18 19.10 -2 -3 -16 179.38 31.50 -2 -3 -16 183.98 21.20 2 3 16 180.98 19.20 2 3 16 248.38 27.20 2 3 16 108.29 23.90 -3 -3 -16 41.50 14.30 -3 -3 -16 53.39 11.60 -3 -3 -16 55.09 14.20 3 3 16 60.49 22.20 3 3 16 86.59 15.40 3 3 16 23.10 17.00 3 3 16 51.99 15.50 3 3 16 73.49 13.80 2 -4 -16 43.20 22.20 2 -4 -16 4.60 9.00 2 -4 -16 20.40 10.70 -2 4 16 22.10 15.30 -2 4 16 23.90 8.90 -2 4 16 11.60 8.70 1 -4 -16 207.18 29.40 1 -4 -16 155.78 17.80 1 -4 -16 197.28 19.50 -1 4 16 164.78 16.70 -1 4 16 186.08 22.30 0 -4 -16 38.80 11.60 0 -4 -16 28.30 9.90 0 -4 -16 40.70 19.90 0 -4 -16 14.40 11.60 0 4 16 37.40 10.30 0 4 16 31.30 9.80 0 4 16 23.70 13.80 -1 -4 -16 201.98 18.80 -1 -4 -16 199.38 30.40 -1 -4 -16 187.68 20.20 -1 -4 -16 177.18 21.00 1 4 16 217.88 23.70 1 4 16 221.18 18.40 1 4 16 190.48 24.20 1 4 16 229.48 18.00 1 4 16 192.28 17.90 -2 -4 -16 167.08 28.40 -2 -4 -16 173.98 19.30 -2 -4 -16 121.99 19.00 -2 -4 -16 140.69 16.40 2 4 16 168.08 18.00 2 4 16 208.28 24.60 2 4 16 148.79 19.70 -3 -4 -16 67.69 13.10 -3 -4 -16 38.80 13.80 -3 -4 -16 71.29 16.00 3 4 16 35.90 10.90 3 4 16 56.99 13.20 3 4 16 75.19 19.40 3 4 16 50.99 12.60 2 -5 -16 61.39 13.20 2 -5 -16 43.40 12.10 -2 5 16 27.70 15.70 -2 5 16 41.90 11.00 -2 5 16 53.59 10.60 1 -5 -16 93.09 14.00 1 -5 -16 148.59 25.60 1 -5 -16 82.39 14.60 -1 5 16 76.49 17.40 -1 5 16 85.59 12.60 0 -5 -16 6.70 15.70 0 -5 -16 -1.90 10.70 0 -5 -16 -2.40 6.60 0 -5 -16 -1.40 7.20 0 5 16 10.30 13.40 0 5 16 0.60 5.80 0 5 16 7.30 7.10 -1 -5 -16 247.68 22.10 -1 -5 -16 233.38 23.00 -1 -5 -16 256.97 20.30 1 5 16 241.78 17.70 1 5 16 197.38 25.00 1 5 16 276.17 20.20 1 5 16 221.68 19.20 -2 -5 -16 116.99 15.90 -2 -5 -16 95.29 16.70 -2 -5 -16 121.79 19.20 2 5 16 97.69 18.50 2 5 16 137.89 15.90 2 5 16 139.89 16.10 -3 -5 -16 72.69 12.00 -3 -5 -16 61.29 15.20 -3 -5 -16 56.49 14.70 3 5 16 114.09 24.00 3 5 16 88.79 15.50 3 5 16 88.39 14.90 3 5 16 115.79 17.50 2 -6 -16 168.18 19.10 -2 6 16 211.88 22.80 -2 6 16 175.38 17.20 -2 6 16 166.78 16.50 1 -6 -16 8.60 8.80 1 -6 -16 8.00 7.90 1 -6 -16 26.40 16.80 1 -6 -16 19.00 11.60 -1 6 16 15.40 11.30 -1 6 16 10.00 13.40 0 -6 -16 259.57 20.40 0 -6 -16 272.07 27.90 0 -6 -16 232.78 22.90 0 6 16 258.57 19.40 0 6 16 232.78 25.40 0 6 16 246.88 19.70 -1 -6 -16 5.90 10.30 -1 -6 -16 -0.50 6.50 -1 -6 -16 12.80 8.40 1 6 16 7.00 7.30 1 6 16 6.90 6.90 1 6 16 -1.00 11.10 -2 -6 -16 223.18 19.20 -2 -6 -16 241.88 23.00 -2 -6 -16 226.98 22.20 2 6 16 275.77 19.80 2 6 16 263.57 21.60 2 6 16 248.88 20.70 2 6 16 223.08 28.20 -3 -6 -16 7.50 11.00 -3 -6 -16 10.80 9.90 3 6 16 15.00 17.60 3 6 16 43.70 18.30 3 6 16 18.30 9.70 3 6 16 10.00 10.70 2 -7 -16 3.90 8.10 2 -7 -16 37.00 19.60 2 -7 -16 11.00 9.50 -2 7 16 8.40 8.70 -2 7 16 37.10 14.90 -2 7 16 18.20 7.60 1 -7 -16 149.99 18.70 1 -7 -16 183.18 25.20 1 -7 -16 179.88 17.50 1 -7 -16 146.99 19.90 -1 7 16 175.98 23.20 -1 7 16 158.98 14.90 0 -7 -16 5.40 8.10 0 -7 -16 38.20 12.60 0 -7 -16 44.00 10.10 0 7 16 34.80 10.10 0 7 16 26.50 13.80 0 7 16 42.80 9.70 -1 -7 -16 70.39 22.60 -1 -7 -16 60.69 13.90 -1 -7 -16 70.19 12.00 1 7 16 91.79 13.60 1 7 16 58.89 18.70 1 7 16 80.99 12.80 -2 -7 -16 105.69 14.00 -2 -7 -16 154.98 21.10 -2 -7 -16 157.48 19.00 2 7 16 175.68 15.40 2 7 16 102.99 21.70 2 7 16 151.28 19.30 2 7 16 157.38 17.30 -3 -7 -16 25.90 9.30 -3 -7 -16 58.19 13.60 3 7 16 29.00 10.30 3 7 16 40.00 11.10 2 -8 -16 61.29 23.10 2 -8 -16 43.00 10.90 2 -8 -16 50.09 12.30 -2 8 16 49.50 11.40 -2 8 16 39.10 8.50 -2 8 16 62.19 17.40 1 -8 -16 96.69 14.20 1 -8 -16 81.09 15.50 1 -8 -16 92.29 14.90 -1 8 16 106.59 12.20 -1 8 16 169.88 22.50 0 -8 -16 200.38 17.90 0 -8 -16 212.58 20.80 0 -8 -16 183.78 19.00 0 8 16 185.68 17.20 0 8 16 242.68 26.40 0 8 16 204.68 16.60 -1 -8 -16 262.27 22.60 -1 -8 -16 253.07 23.50 -1 -8 -16 282.97 20.80 1 8 16 317.17 20.80 -2 -8 -16 22.50 11.10 -2 -8 -16 42.90 12.70 -2 -8 -16 23.40 8.40 2 8 16 13.10 16.10 2 8 16 22.80 8.50 2 8 16 43.10 11.60 2 8 16 13.30 8.20 -3 -8 -16 115.99 15.70 -3 -8 -16 128.69 19.70 -3 -8 -16 144.09 20.10 3 8 16 107.29 15.70 2 -9 -16 259.47 31.60 1 -9 -16 8.00 8.20 1 -9 -16 11.60 11.40 1 -9 -16 20.90 8.60 -1 9 16 5.80 14.50 -1 9 16 18.60 16.90 -1 9 16 19.70 6.50 0 -9 -16 30.20 9.90 0 -9 -16 33.30 11.80 0 -9 -16 53.79 10.80 0 9 16 42.40 18.60 0 9 16 52.49 9.20 0 9 16 47.20 10.40 -1 -9 -16 10.60 10.50 -1 -9 -16 10.20 8.60 -1 -9 -16 11.70 7.60 1 9 16 3.10 8.10 1 9 16 10.40 15.60 1 9 16 7.10 6.20 -2 -9 -16 34.70 8.70 -2 -9 -16 17.50 13.50 -2 -9 -16 33.60 11.00 2 9 16 43.20 8.90 2 9 16 37.20 9.70 2 9 16 34.20 9.00 2 9 16 25.00 18.10 1 -10 -16 112.19 14.70 1 -10 -16 92.39 12.90 1 -10 -16 90.49 16.10 -1 10 16 141.29 21.30 -1 10 16 129.89 18.50 -1 10 16 106.89 11.00 0 -10 -16 2.00 7.10 0 -10 -16 1.70 6.60 0 -10 -16 -11.80 9.00 0 10 16 0.00 7.70 0 10 16 3.20 5.30 0 10 16 -13.50 17.50 -1 -10 -16 6.20 10.30 -1 -10 -16 8.80 7.00 -1 -10 -16 6.30 7.70 1 10 16 5.30 7.10 1 10 16 5.10 15.80 1 10 16 -0.40 5.50 -2 -10 -16 156.98 20.00 -2 -10 -16 151.08 17.00 2 10 16 196.28 15.40 2 10 16 161.88 17.50 2 10 16 206.28 19.30 0 -11 -16 17.30 8.10 0 -11 -16 24.60 11.40 0 -11 -16 12.70 8.90 0 11 16 23.40 6.70 0 11 16 19.20 18.80 0 11 16 34.80 16.30 -1 -11 -16 215.78 19.50 -1 -11 -16 198.28 17.30 1 11 16 208.58 17.60 1 11 16 214.68 16.00 0 0 -17 100.29 16.30 0 0 -17 124.39 18.30 0 0 17 144.29 16.80 0 0 17 131.99 16.50 0 0 17 174.68 27.40 0 0 17 125.79 18.00 -1 0 -17 29.20 30.60 -1 0 -17 13.90 9.90 1 0 17 -0.50 8.40 1 0 17 2.70 8.30 1 0 17 -6.40 16.40 1 -1 -17 196.08 20.50 1 -1 -17 222.88 37.60 -1 1 17 195.98 16.50 -1 1 17 174.58 18.40 0 -1 -17 52.79 12.90 0 -1 -17 50.09 28.90 0 -1 -17 37.00 11.90 0 1 17 51.19 18.80 0 1 17 38.20 18.70 0 1 17 17.80 21.20 0 1 17 42.40 10.90 0 1 17 43.20 11.30 -1 -1 -17 -0.50 8.20 -1 -1 -17 -0.30 8.40 1 1 17 3.70 16.00 1 1 17 -2.70 6.70 1 1 17 -1.70 6.70 1 1 17 -4.40 18.50 -2 -1 -17 239.98 42.60 2 1 17 181.48 27.80 2 1 17 226.38 35.30 1 -2 -17 40.00 11.60 1 -2 -17 12.60 12.90 -1 2 17 34.00 13.00 -1 2 17 38.80 9.80 -1 2 17 78.89 20.00 0 -2 -17 2.80 8.30 0 -2 -17 29.90 21.70 0 -2 -17 -1.60 7.10 0 2 17 -1.30 8.10 0 2 17 1.90 7.30 0 2 17 2.30 15.20 0 2 17 17.10 9.60 0 2 17 4.10 13.00 -1 -2 -17 192.28 35.30 -1 -2 -17 176.78 18.70 1 2 17 154.28 17.00 1 2 17 112.99 22.70 1 2 17 149.49 16.80 -2 -2 -17 33.90 12.20 -2 -2 -17 42.60 25.00 -2 -2 -17 29.10 10.20 2 2 17 14.30 8.90 2 2 17 13.70 9.00 2 2 17 35.70 19.50 1 -3 -17 5.50 8.50 1 -3 -17 5.70 9.00 1 -3 -17 19.50 22.60 -1 3 17 6.20 8.00 -1 3 17 4.50 15.70 -1 3 17 9.10 7.40 0 -3 -17 329.97 25.20 0 -3 -17 310.37 26.50 0 -3 -17 412.76 39.90 0 3 17 337.87 23.90 0 3 17 343.57 29.90 0 3 17 312.97 24.40 -1 -3 -17 141.99 18.30 -1 -3 -17 122.79 18.40 -1 -3 -17 163.68 31.50 1 3 17 147.39 16.60 1 3 17 118.89 23.10 1 3 17 176.58 23.90 1 3 17 148.99 16.80 -2 -3 -17 196.38 26.50 -2 -3 -17 189.48 20.00 -2 -3 -17 249.18 33.20 2 3 17 123.09 24.40 2 3 17 210.18 19.80 2 3 17 231.48 22.10 2 3 17 209.48 20.10 2 -4 -17 15.20 22.70 1 -4 -17 24.20 11.10 1 -4 -17 52.69 11.40 1 -4 -17 79.89 23.40 -1 4 17 36.00 10.10 -1 4 17 50.09 10.60 -1 4 17 31.40 17.80 0 -4 -17 314.67 35.20 0 -4 -17 279.17 24.60 0 -4 -17 285.57 22.80 0 4 17 258.67 20.90 0 4 17 285.67 28.90 0 4 17 299.97 22.20 -1 -4 -17 33.50 12.80 -1 -4 -17 57.19 12.00 -1 -4 -17 77.19 26.60 -1 -4 -17 35.70 11.60 1 4 17 51.59 12.10 1 4 17 48.80 15.30 1 4 17 70.79 19.00 1 4 17 44.50 11.40 1 4 17 7.00 15.00 -2 -4 -17 82.69 13.70 -2 -4 -17 89.29 18.10 -2 -4 -17 75.89 16.40 -2 -4 -17 104.59 25.10 2 4 17 101.49 16.60 2 4 17 51.29 17.90 2 4 17 108.19 21.10 2 4 17 77.19 14.70 2 -5 -17 104.69 17.40 -2 5 17 102.79 14.50 1 -5 -17 85.39 15.80 1 -5 -17 81.49 13.90 -1 5 17 75.19 17.90 -1 5 17 135.89 15.50 0 -5 -17 -6.10 7.70 0 -5 -17 2.60 7.50 0 -5 -17 14.90 17.90 0 -5 -17 3.40 10.50 0 5 17 -5.20 14.70 0 5 17 -1.00 12.50 0 5 17 4.40 7.10 -1 -5 -17 242.98 24.50 -1 -5 -17 250.87 21.70 -1 -5 -17 244.58 23.60 -1 -5 -17 311.57 34.90 1 5 17 231.98 28.00 1 5 17 265.17 20.70 1 5 17 304.27 19.50 1 5 17 272.47 22.00 -2 -5 -17 -3.90 6.60 -2 -5 -17 0.30 10.60 -2 -5 -17 -1.20 8.50 2 5 17 4.30 14.40 2 5 17 -4.70 6.20 2 5 17 2.10 9.10 2 5 17 -1.80 6.90 1 -6 -17 2.00 7.60 1 -6 -17 1.90 9.20 1 -6 -17 35.30 18.90 -1 6 17 0.70 7.10 -1 6 17 5.60 6.50 0 -6 -17 372.96 30.00 0 -6 -17 443.76 28.00 0 -6 -17 411.86 29.90 0 6 17 446.06 27.80 0 6 17 497.25 27.50 0 6 17 362.26 37.80 -1 -6 -17 79.59 12.70 -1 -6 -17 101.89 17.70 -1 -6 -17 78.79 15.70 1 6 17 84.79 19.80 1 6 17 105.79 14.90 -2 -6 -17 33.20 14.50 -2 -6 -17 54.79 13.00 -2 -6 -17 59.69 11.80 2 6 17 54.89 11.40 2 6 17 48.40 11.50 2 6 17 56.89 12.80 2 6 17 15.20 17.90 1 -7 -17 123.49 23.00 1 -7 -17 100.19 17.00 1 -7 -17 92.89 14.10 1 -7 -17 134.49 24.90 -1 7 17 132.89 15.10 0 -7 -17 28.90 9.30 0 -7 -17 28.50 10.60 0 -7 -17 13.60 12.70 0 7 17 20.80 18.80 0 7 17 28.70 9.30 0 7 17 36.50 9.30 -1 -7 -17 115.99 17.90 -1 -7 -17 120.69 17.40 -1 -7 -17 157.78 16.30 1 7 17 152.78 15.80 1 7 17 147.09 16.60 1 7 17 141.29 24.60 -2 -7 -17 154.28 33.10 -2 -7 -17 208.28 25.70 2 7 17 204.88 23.50 2 7 17 162.68 18.30 2 7 17 176.98 32.70 2 7 17 223.58 17.50 1 -8 -17 147.89 19.70 1 -8 -17 171.48 19.10 1 -8 -17 157.28 17.50 -1 8 17 174.88 17.00 -1 8 17 151.98 14.80 0 -8 -17 -2.20 10.30 0 -8 -17 -1.00 7.20 0 -8 -17 -0.30 7.90 0 8 17 -1.80 5.80 0 8 17 -1.30 7.00 0 8 17 -0.50 15.80 -1 -8 -17 156.58 20.70 -1 -8 -17 126.89 18.90 -1 -8 -17 141.49 16.70 1 8 17 115.09 23.00 1 8 17 149.79 15.20 1 8 17 135.89 18.20 -2 -8 -17 5.90 7.10 -2 -8 -17 -4.20 7.80 -2 -8 -17 4.50 10.80 2 8 17 5.00 7.70 1 -9 -17 5.10 11.40 1 -9 -17 22.00 9.80 -1 9 17 31.60 9.40 -1 9 17 4.40 17.40 -1 9 17 12.10 6.80 0 -9 -17 228.88 19.20 0 -9 -17 203.38 21.60 0 -9 -17 165.58 19.50 0 9 17 305.67 29.90 0 9 17 244.88 17.30 0 9 17 232.38 19.40 -1 -9 -17 1.50 8.40 -1 -9 -17 -0.60 8.20 -1 -9 -17 -14.30 10.70 1 9 17 -0.20 6.00 1 9 17 9.60 8.70 1 9 17 2.90 15.60 -2 -9 -17 -9.00 8.80 -2 -9 -17 9.50 7.40 2 9 17 4.90 7.50 0 -10 -17 99.49 14.10 0 -10 -17 132.29 18.30 0 -10 -17 70.59 15.30 0 10 17 132.79 16.40 0 10 17 114.79 11.90 -1 -10 -17 107.19 15.50 -1 -10 -17 79.29 13.90 -1 -10 -17 69.09 15.70 1 10 17 86.79 12.50 1 10 17 115.99 15.50 0 -2 -18 29.00 26.90 0 -3 -18 65.99 15.30 0 -3 -18 197.28 51.29 0 3 18 88.49 13.40 -1 -3 -18 9.90 13.50 -1 -3 -18 49.70 12.80 -1 -3 -18 63.39 28.70 1 3 18 70.79 18.70 1 3 18 20.70 9.00 1 -4 -18 80.49 33.40 0 -4 -18 23.70 11.40 0 -4 -18 12.30 11.00 0 -4 -18 31.20 24.10 0 4 18 8.90 7.50 -1 -4 -18 7.00 10.50 -1 -4 -18 6.00 12.50 -1 -4 -18 17.00 11.30 -1 -4 -18 6.10 24.10 1 4 18 15.50 10.10 1 4 18 15.80 12.80 1 4 18 -1.20 7.50 1 -5 -18 65.49 14.80 1 -5 -18 102.69 23.90 -1 5 18 44.50 10.30 -1 5 18 48.10 19.90 0 -5 -18 4.20 12.20 0 -5 -18 24.00 11.50 0 -5 -18 7.70 21.90 0 5 18 7.40 7.30 0 5 18 15.40 16.50 -1 -5 -18 202.08 26.80 -1 -5 -18 195.78 26.90 -1 -5 -18 213.18 34.00 -1 -5 -18 203.98 21.40 1 5 18 183.98 18.30 1 5 18 216.48 19.20 1 -6 -18 4.20 10.10 1 -6 -18 31.50 18.80 -1 6 18 0.90 8.30 0 -6 -18 35.30 11.10 0 -6 -18 33.50 15.70 0 -6 -18 36.00 11.60 0 6 18 30.80 9.50 0 6 18 68.49 19.20 -1 -6 -18 48.00 16.60 -1 -6 -18 75.29 14.90 -1 -6 -18 29.90 10.70 1 6 18 53.39 11.10 0 -7 -18 89.19 14.00 0 -7 -18 88.39 16.10 0 -7 -18 55.39 18.10 0 7 18 97.79 22.50 0 7 18 78.69 12.40 -1 -7 -18 -0.90 6.70 -1 -7 -18 -8.90 10.10 -1 -7 -18 -2.50 7.80 1 7 18 3.50 6.70 0 -8 -18 1.00 7.20 0 -8 -18 -1.40 8.60 0 8 18 12.00 6.60 0 8 18 -6.60 19.30 -1 -8 -18 36.00 10.00 -1 -8 -18 28.20 13.30 -1 -8 -18 24.30 11.40 1 8 18 34.20 9.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 29664 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 -0.27688(6) 0.16413(3) 0.96951(2) 0.02107(11) Uani d . . . 1 . . N N1 0.4469(5) 0.3033(2) 0.34605(16) 0.0140(5) Uani d . . . 1 . . O O1 0.5242(4) 0.5187(2) 0.31450(14) 0.0178(4) Uani d . . . 1 . . O O2 0.4853(4) 0.1066(2) 0.32879(15) 0.0194(5) Uani d . . . 1 . . C C1 0.2360(6) 0.2741(3) 0.4271(2) 0.0146(6) Uani d . . . 1 . . C C2 0.2098(6) 0.1492(3) 0.4968(2) 0.0166(6) Uani d . . . 1 . . H H2 0.329733 0.083735 0.490592 0.02 Uiso calc U . R 1 . . C C3 0.0056(6) 0.1218(3) 0.5754(2) 0.0159(6) Uani d . . . 1 . . H H3 -0.01569 0.036648 0.621565 0.019 Uiso calc U . R 1 . . C C4 -0.1657(6) 0.2158(3) 0.5872(2) 0.0148(6) Uani d . . . 1 . . C C5 -0.1370(6) 0.3396(3) 0.5173(2) 0.0153(6) Uani d . . . 1 . . H H5 -0.25483 0.405115 0.524375 0.018 Uiso calc U . R 1 . . C C6 0.0619(6) 0.3691(3) 0.4370(2) 0.0155(6) Uani d . . . 1 . . H H6 0.077633 0.453745 0.389496 0.019 Uiso calc U . R 1 . . C C7 -0.3774(6) 0.1878(3) 0.6756(2) 0.0155(6) Uani d . . . 1 . . H H7A -0.522126 0.255745 0.659896 0.019 Uiso calc U . R 1 . . H H7B -0.472483 0.106345 0.688149 0.019 Uiso calc U . R 1 . . C C8 -0.2421(6) 0.1791(3) 0.7685(2) 0.0161(6) Uani d . . . 1 . . F F1 -0.0729(3) 0.07242(16) 0.80056(12) 0.0211(4) Uani d . . . 1 . . F F2 -0.0606(3) 0.27967(16) 0.74733(12) 0.0183(4) Uani d . . . 1 . . C C9 -0.4552(6) 0.1774(3) 0.8504(2) 0.0186(6) Uani d . . . 1 . . H H9A -0.583073 0.10431 0.866293 0.022 Uiso calc U . R 1 . . H H9B -0.569404 0.256298 0.827539 0.022 Uiso calc U . R 1 . . C C10 0.5768(6) 0.4243(3) 0.2982(2) 0.0150(6) Uani d . . . 1 . . C C11 0.7952(6) 0.4079(3) 0.2248(2) 0.0147(6) Uani d . . . 1 . . C C12 0.9854(6) 0.4954(3) 0.1610(2) 0.0174(6) Uani d . . . 1 . . H H12 0.989826 0.580553 0.157526 0.021 Uiso calc U . R 1 . . C C13 1.1705(6) 0.4522(3) 0.1021(2) 0.0200(7) Uani d . . . 1 . . H H13 1.304975 0.509291 0.057416 0.024 Uiso calc U . R 1 . . C C14 1.1628(6) 0.3277(3) 0.1072(2) 0.0196(6) Uani d . . . 1 . . H H14 1.291713 0.301354 0.065901 0.024 Uiso calc U . R 1 . . C C15 0.9686(6) 0.2405(3) 0.1719(2) 0.0176(6) Uani d . . . 1 . . H H15 0.96223 0.155243 0.175623 0.021 Uiso calc U . R 1 . . C C16 0.7867(6) 0.2838(3) 0.2302(2) 0.0155(6) Uani d . . . 1 . . C C17 0.5605(6) 0.2153(3) 0.3061(2) 0.0151(6) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.02430(17) 0.02291(19) 0.01763(16) -0.00478(12) -0.00035(11) -0.00933(12) N1 0.0149(11) 0.0124(13) 0.0159(11) -0.0016(10) 0.0000(9) -0.0067(9) O1 0.0178(10) 0.0128(11) 0.0246(11) -0.0025(9) 0.0009(8) -0.0095(8) O2 0.0214(11) 0.0145(12) 0.0252(11) -0.0048(9) 0.0017(8) -0.0110(9) C1 0.0130(13) 0.0149(16) 0.0187(14) -0.0011(12) -0.0013(11) -0.0096(11) C2 0.0170(14) 0.0130(16) 0.0208(14) 0.0003(12) -0.0004(11) -0.0076(12) C3 0.0155(14) 0.0133(15) 0.0192(14) -0.0029(12) -0.0010(11) -0.0061(11) C4 0.0118(13) 0.0177(16) 0.0178(14) -0.0062(12) -0.0018(11) -0.0093(11) C5 0.0134(13) 0.0147(15) 0.0232(15) 0.0018(12) -0.0033(11) -0.0131(12) C6 0.0154(14) 0.0139(15) 0.0192(14) -0.0012(12) -0.0049(11) -0.0075(11) C7 0.0124(13) 0.0142(15) 0.0218(15) -0.0028(11) 0.0003(11) -0.0093(11) C8 0.0153(13) 0.0106(15) 0.0242(15) -0.0008(12) -0.0009(11) -0.0086(12) F1 0.0221(9) 0.0173(10) 0.0261(9) 0.0056(7) -0.0043(7) -0.0105(7) F2 0.0162(8) 0.0184(9) 0.0224(9) -0.0075(7) 0.0012(6) -0.0101(7) C9 0.0154(14) 0.0223(17) 0.0188(14) -0.0032(12) -0.0004(11) -0.0085(12) C10 0.0132(13) 0.0156(16) 0.0162(14) -0.0007(12) -0.0050(11) -0.0051(11) C11 0.0127(13) 0.0167(16) 0.0158(13) 0.0010(12) -0.0045(10) -0.0067(11) C12 0.0167(14) 0.0183(16) 0.0180(14) -0.0023(12) -0.0018(11) -0.0075(12) C13 0.0148(14) 0.0259(18) 0.0203(15) -0.0027(13) 0.0000(11) -0.0097(12) C14 0.0146(14) 0.0276(18) 0.0185(14) 0.0023(13) -0.0011(11) -0.0109(12) C15 0.0186(14) 0.0167(16) 0.0201(14) 0.0014(12) -0.0033(11) -0.0096(12) C16 0.0138(13) 0.0171(16) 0.0153(13) -0.0006(12) -0.0038(11) -0.0053(11) C17 0.0125(13) 0.0161(16) 0.0181(14) -0.0009(12) -0.0026(11) -0.0079(11) 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' Br Br -0.2901 2.4595 '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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C17 N1 C10 . . 110.9(2) ? C17 N1 C1 . . 124.9(2) ? C10 N1 C1 . . 124.1(2) ? C6 C1 C2 . . 120.0(3) ? C6 C1 N1 . . 120.3(3) ? C2 C1 N1 . . 119.7(3) ? C3 C2 C1 . . 119.3(3) ? C3 C2 H2 . . 120.3 ? C1 C2 H2 . . 120.3 ? C4 C3 C2 . . 121.3(3) ? C4 C3 H3 . . 119.3 ? C2 C3 H3 . . 119.3 ? C3 C4 C5 . . 118.6(3) ? C3 C4 C7 . . 121.5(3) ? C5 C4 C7 . . 119.9(3) ? C4 C5 C6 . . 121.2(3) ? C4 C5 H5 . . 119.4 ? C6 C5 H5 . . 119.4 ? C1 C6 C5 . . 119.5(3) ? C1 C6 H6 . . 120.2 ? C5 C6 H6 . . 120.2 ? C8 C7 C4 . . 112.5(2) ? C8 C7 H7A . . 109.1 ? C4 C7 H7A . . 109.1 ? C8 C7 H7B . . 109.1 ? C4 C7 H7B . . 109.1 ? H7A C7 H7B . . 107.8 ? F1 C8 F2 . . 104.5(2) ? F1 C8 C9 . . 110.0(2) ? F2 C8 C9 . . 109.3(2) ? F1 C8 C7 . . 110.0(2) ? F2 C8 C7 . . 110.1(2) ? C9 C8 C7 . . 112.6(2) ? C8 C9 Br1 . . 111.88(19) ? C8 C9 H9A . . 109.2 ? Br1 C9 H9A . . 109.2 ? C8 C9 H9B . . 109.2 ? Br1 C9 H9B . . 109.2 ? H9A C9 H9B . . 107.9 ? O1 C10 N1 . . 126.9(3) ? O1 C10 C11 . . 127.5(3) ? N1 C10 C11 . . 105.6(2) ? C16 C11 C12 . . 122.1(3) ? C16 C11 C10 . . 108.7(2) ? C12 C11 C10 . . 129.2(3) ? C11 C12 C13 . . 116.6(3) ? C11 C12 H12 . . 121.7 ? C13 C12 H12 . . 121.7 ? C14 C13 C12 . . 121.5(3) ? C14 C13 H13 . . 119.2 ? C12 C13 H13 . . 119.2 ? C13 C14 C15 . . 121.2(3) ? C13 C14 H14 . . 119.4 ? C15 C14 H14 . . 119.4 ? C16 C15 C14 . . 117.0(3) ? C16 C15 H15 . . 121.5 ? C14 C15 H15 . . 121.5 ? C15 C16 C11 . . 121.6(3) ? C15 C16 C17 . . 129.9(3) ? C11 C16 C17 . . 108.4(3) ? O2 C17 N1 . . 126.3(3) ? O2 C17 C16 . . 127.4(3) ? N1 C17 C16 . . 106.3(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C9 . 1.952(3) ? N1 C17 . 1.413(4) ? N1 C10 . 1.422(4) ? N1 C1 . 1.441(3) ? O1 C10 . 1.199(4) ? O2 C17 . 1.208(4) ? C1 C6 . 1.384(4) ? C1 C2 . 1.402(4) ? C2 C3 . 1.397(4) ? C2 H2 . 0.95 ? C3 C4 . 1.379(4) ? C3 H3 . 0.95 ? C4 C5 . 1.394(4) ? C4 C7 . 1.520(4) ? C5 C6 . 1.397(4) ? C5 H5 . 0.95 ? C6 H6 . 0.95 ? C7 C8 . 1.518(4) ? C7 H7A . 0.99 ? C7 H7B . 0.99 ? C8 F1 . 1.379(3) ? C8 F2 . 1.381(3) ? C8 C9 . 1.508(4) ? C9 H9A . 0.99 ? C9 H9B . 0.99 ? C10 C11 . 1.498(4) ? C11 C16 . 1.382(4) ? C11 C12 . 1.383(4) ? C12 C13 . 1.394(4) ? C12 H12 . 0.95 ? C13 C14 . 1.389(5) ? C13 H13 . 0.95 ? C14 C15 . 1.398(4) ? C14 H14 . 0.95 ? C15 C16 . 1.380(4) ? C15 H15 . 0.95 ? C16 C17 . 1.492(4) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C17 N1 C1 C6 . . . . -154.9(3) ? C10 N1 C1 C6 . . . . 27.7(4) ? C17 N1 C1 C2 . . . . 25.9(4) ? C10 N1 C1 C2 . . . . -151.4(3) ? C6 C1 C2 C3 . . . . 0.5(4) ? N1 C1 C2 C3 . . . . 179.7(2) ? C1 C2 C3 C4 . . . . -1.8(4) ? C2 C3 C4 C5 . . . . 1.8(4) ? C2 C3 C4 C7 . . . . -176.7(2) ? C3 C4 C5 C6 . . . . -0.5(4) ? C7 C4 C5 C6 . . . . 178.0(2) ? C2 C1 C6 C5 . . . . 0.7(4) ? N1 C1 C6 C5 . . . . -178.5(2) ? C4 C5 C6 C1 . . . . -0.7(4) ? C3 C4 C7 C8 . . . . 78.8(3) ? C5 C4 C7 C8 . . . . -99.6(3) ? C4 C7 C8 F1 . . . . -68.3(3) ? C4 C7 C8 F2 . . . . 46.3(3) ? C4 C7 C8 C9 . . . . 168.6(3) ? F1 C8 C9 Br1 . . . . 56.3(3) ? F2 C8 C9 Br1 . . . . -57.9(3) ? C7 C8 C9 Br1 . . . . 179.31(19) ? C17 N1 C10 O1 . . . . 179.0(3) ? C1 N1 C10 O1 . . . . -3.3(4) ? C17 N1 C10 C11 . . . . -1.9(3) ? C1 N1 C10 C11 . . . . 175.7(2) ? O1 C10 C11 C16 . . . . 179.7(3) ? N1 C10 C11 C16 . . . . 0.7(3) ? O1 C10 C11 C12 . . . . 0.9(5) ? N1 C10 C11 C12 . . . . -178.1(3) ? C16 C11 C12 C13 . . . . -0.2(4) ? C10 C11 C12 C13 . . . . 178.5(3) ? C11 C12 C13 C14 . . . . 0.2(4) ? C12 C13 C14 C15 . . . . -0.1(4) ? C13 C14 C15 C16 . . . . -0.1(4) ? C14 C15 C16 C11 . . . . 0.1(4) ? C14 C15 C16 C17 . . . . -179.5(3) ? C12 C11 C16 C15 . . . . 0.0(4) ? C10 C11 C16 C15 . . . . -178.9(2) ? C12 C11 C16 C17 . . . . 179.7(2) ? C10 C11 C16 C17 . . . . 0.8(3) ? C10 N1 C17 O2 . . . . -176.9(3) ? C1 N1 C17 O2 . . . . 5.4(4) ? C10 N1 C17 C16 . . . . 2.4(3) ? C1 N1 C17 C16 . . . . -175.3(2) ? C15 C16 C17 O2 . . . . -3.0(5) ? C11 C16 C17 O2 . . . . 177.4(3) ? C15 C16 C17 N1 . . . . 177.7(3) ? C11 C16 C17 N1 . . . . -1.9(3) ?