#------------------------------------------------------------------------------ #$Date: 2019-04-24 05:30:58 +0300 (Wed, 24 Apr 2019) $ #$Revision: 214746 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/29/2242911.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2242911 loop_ _publ_author_name 'Khalilov, Ali N.' 'Atio\(glu, Zeliha' 'Akkurt, Mehmet' 'Duruskari, Gulnara Sh.' 'Toze, Flavien A. A.' 'Huseynova, Afet T.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (E)-3-[(4-fluorobenzylidene)amino]-5-phenylthiazolidin-2-iminium bromide ; _journal_coeditor_code RZ5254 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 662 _journal_page_last 666 _journal_paper_doi 10.1107/S2056989019004973 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C16 H15 F1 N3 S1 +, Br -' _chemical_formula_moiety 'C16 H15 F1 N3 S1 +, Br -' _chemical_formula_sum 'C16 H15 Br F N3 S' _chemical_formula_weight 380.28 _chemical_name_systematic ; (E)-3-[(4-Fluorobenzylidene)amino]-5-phenylthiazolidin-2-iminium bromide ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 96.548(2) _cell_angle_beta 92.518(2) _cell_angle_gamma 111.065(2) _cell_formula_units_Z 2 _cell_length_a 8.0599(3) _cell_length_b 8.6086(4) _cell_length_c 12.7608(5) _cell_measurement_reflns_used 5655 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.33 _cell_measurement_theta_min 2.56 _cell_volume 817.39(6) _computing_cell_refinement ; SAINT (Bruker, 2007) ; _computing_data_collection ; APEX2 (Bruker, 2007) ; _computing_data_reduction ; SAINT (Bruker, 2007) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; PLATON (Spek, 2003) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12009 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.470 _diffrn_reflns_theta_min 2.720 _exptl_absorpt_coefficient_mu 2.651 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_correction_T_min 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2003) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.545 _exptl_crystal_description plate _exptl_crystal_F_000 384 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.374 _refine_diff_density_min -0.482 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 3321 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0285 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+0.2228P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.0769 _reflns_number_gt 2672 _reflns_number_total 3321 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rz5254sup1.cif _cod_data_source_block I _cod_database_code 2242911 _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 0.676 _shelx_estimated_absorpt_t_max 0.796 _shelx_hkl_file ; -1 0 0 331.97 9.50 -1 0 0 337.87 9.60 -1 0 0 341.97 9.60 -1 0 0 358.86 9.60 1 0 0 336.57 9.50 1 0 0 366.56 9.60 -2 0 0 107.19 3.20 -2 0 0 105.19 3.20 -2 0 0 110.99 3.20 -2 0 0 107.49 3.10 2 0 0 109.59 3.20 2 0 0 113.89 3.20 2 0 0 105.49 3.00 -3 0 0 7.50 0.60 -3 0 0 7.40 0.60 -3 0 0 8.10 0.50 -3 0 0 7.80 0.60 3 0 0 7.60 0.40 3 0 0 7.60 0.60 3 0 0 8.90 0.60 3 0 0 6.60 0.50 -4 0 0 222.78 6.40 -4 0 0 218.78 6.40 -4 0 0 214.68 6.30 -4 0 0 211.28 6.10 4 0 0 210.18 6.30 4 0 0 212.18 6.10 4 0 0 222.48 6.30 4 0 0 223.48 6.40 -5 0 0 373.36 11.00 -5 0 0 392.06 11.10 -5 0 0 386.96 11.00 5 0 0 381.66 10.60 5 0 0 377.06 10.90 -6 0 0 3.00 1.00 -6 0 0 2.20 0.90 -6 0 0 1.10 0.70 6 0 0 2.10 0.40 6 0 0 1.00 0.70 -7 0 0 24.80 1.80 -7 0 0 29.10 1.90 -8 0 0 -1.10 1.20 -8 0 0 -0.90 1.30 -9 0 0 2.20 1.70 -9 0 0 1.10 1.50 -9 1 0 -0.60 1.60 -9 1 0 0.00 1.40 -8 1 0 2.20 1.40 -8 1 0 4.60 1.30 7 -1 0 23.70 1.30 7 -1 0 23.40 1.70 -7 1 0 24.20 1.30 -7 1 0 21.80 1.70 -7 1 0 27.70 2.00 -7 1 0 24.80 1.70 6 -1 0 15.90 0.90 6 -1 0 16.00 1.20 -6 1 0 18.20 1.30 -6 1 0 15.80 1.10 -6 1 0 17.70 1.40 -6 1 0 15.60 1.00 5 -1 0 21.90 1.00 5 -1 0 22.30 1.20 -5 1 0 22.90 1.40 -5 1 0 23.40 1.50 -5 1 0 21.70 1.30 -5 1 0 21.30 1.00 4 -1 0 16.80 1.00 4 -1 0 17.70 0.90 4 -1 0 15.80 0.80 4 -1 0 18.60 1.00 -4 1 0 15.60 1.10 -4 1 0 19.70 1.20 -4 1 0 18.40 0.80 -4 1 0 16.40 1.00 3 -1 0 302.07 8.50 3 -1 0 304.97 8.60 3 -1 0 294.97 8.60 3 -1 0 306.07 8.50 -3 1 0 304.17 8.50 -3 1 0 311.67 8.60 -3 1 0 310.07 8.60 -3 1 0 299.27 8.60 2 -1 0 2308.37 61.89 2 -1 0 2234.78 62.19 2 -1 0 2260.87 61.99 2 -1 0 2255.97 61.89 -2 1 0 2128.19 61.89 -2 1 0 2160.78 61.89 -2 1 0 2288.77 61.99 -2 1 0 2260.17 62.39 1 -1 0 14.60 0.50 1 -1 0 14.90 0.50 1 -1 0 14.80 0.60 -1 1 0 15.70 0.60 -1 1 0 15.60 0.50 -1 1 0 15.60 0.50 0 -1 0 230.28 6.80 0 1 0 266.17 6.90 0 1 0 243.28 6.80 -1 -1 0 8.40 0.60 -1 -1 0 9.40 0.50 1 1 0 7.40 0.50 -2 -1 0 544.95 14.90 -2 -1 0 514.75 14.90 -2 -1 0 515.95 14.90 2 1 0 537.05 14.90 2 1 0 569.24 14.90 2 1 0 517.25 14.80 -3 -1 0 117.19 3.80 -3 -1 0 123.39 3.80 -3 -1 0 120.29 3.80 3 1 0 127.49 3.80 3 1 0 128.39 3.80 3 1 0 125.39 3.50 3 1 0 124.39 3.80 -4 -1 0 2.10 0.80 -4 -1 0 3.30 0.70 -4 -1 0 1.60 0.60 4 1 0 2.50 0.20 4 1 0 0.80 0.30 4 1 0 3.60 0.80 -5 -1 0 74.99 2.90 -5 -1 0 75.59 2.80 -5 -1 0 71.19 2.70 -6 -1 0 29.50 2.20 -6 -1 0 28.60 1.90 -6 -1 0 26.90 1.80 6 1 0 25.80 1.70 -7 -1 0 31.50 2.10 -7 -1 0 31.80 2.10 -8 -1 0 -1.10 1.50 -8 -1 0 -0.40 1.40 -9 -1 0 1.80 1.90 -9 2 0 -0.20 1.30 -9 2 0 0.20 1.50 -8 2 0 7.50 1.40 -8 2 0 10.30 1.40 -8 2 0 7.50 0.90 7 -2 0 0.40 0.60 7 -2 0 0.60 0.70 -7 2 0 0.00 0.60 -7 2 0 0.00 1.00 -7 2 0 0.50 0.80 -7 2 0 1.80 0.90 6 -2 0 16.80 1.10 6 -2 0 16.90 1.10 -6 2 0 18.60 1.20 -6 2 0 16.90 1.30 -6 2 0 19.50 1.40 -6 2 0 16.30 1.20 5 -2 0 195.88 5.80 5 -2 0 201.48 5.80 -5 2 0 204.28 5.90 -5 2 0 196.68 6.10 -5 2 0 200.38 5.80 -5 2 0 206.78 6.00 4 -2 0 13.40 1.00 4 -2 0 14.60 0.80 4 -2 0 12.90 0.90 4 -2 0 14.30 0.80 -4 2 0 16.10 1.00 -4 2 0 13.10 0.90 -4 2 0 13.10 0.90 -4 2 0 14.20 1.00 3 -2 0 1367.66 38.20 3 -2 0 1390.86 38.30 3 -2 0 1411.56 38.30 3 -2 0 1414.46 38.40 -3 2 0 1386.76 38.50 -3 2 0 1377.36 38.50 -3 2 0 1402.76 38.70 -3 2 0 1359.36 38.60 2 -2 0 65.59 1.90 2 -2 0 62.89 2.00 2 -2 0 69.29 1.90 -2 2 0 61.39 2.00 -2 2 0 59.79 1.90 -2 2 0 61.49 2.00 -2 2 0 60.69 1.90 1 -2 0 1260.97 35.40 1 -2 0 1256.07 35.40 1 -2 0 1255.57 35.20 -1 2 0 1253.57 35.30 -1 2 0 1287.87 35.70 -1 2 0 1337.27 35.50 -1 2 0 1287.37 35.70 0 -2 0 4.00 0.30 0 -2 0 4.30 0.40 0 -2 0 4.30 0.30 0 -2 0 3.50 0.30 0 2 0 4.10 0.30 0 2 0 3.00 0.40 0 2 0 3.80 0.30 0 2 0 2.90 0.40 -1 -2 0 948.61 25.20 -1 -2 0 936.61 25.10 -1 -2 0 925.31 25.20 1 2 0 859.01 25.20 1 2 0 902.11 25.20 1 2 0 891.71 25.10 1 2 0 902.11 25.20 -2 -2 0 643.84 17.60 -2 -2 0 587.74 17.60 -2 -2 0 609.64 17.60 2 2 0 639.94 17.60 2 2 0 649.43 17.60 2 2 0 645.34 17.40 -3 -2 0 2.20 0.60 -3 -2 0 1.50 0.70 -3 -2 0 0.50 0.60 3 2 0 1.70 0.60 3 2 0 -0.20 0.50 3 2 0 0.60 0.60 3 2 0 1.20 0.30 -4 -2 0 764.02 21.80 -4 -2 0 775.12 21.80 -4 -2 0 797.62 21.80 4 2 0 762.62 21.70 -5 -2 0 6.10 1.10 -5 -2 0 6.10 1.00 -5 -2 0 6.20 1.10 5 2 0 6.10 0.90 -6 -2 0 33.60 2.30 -6 -2 0 36.50 2.50 -7 -2 0 6.90 1.50 -7 -2 0 7.00 1.60 -8 -2 0 4.00 1.70 -8 -2 0 6.20 1.70 -10 3 0 1.80 1.80 -10 3 0 -0.70 1.40 -9 3 0 0.00 1.50 -9 3 0 -0.40 1.20 -8 3 0 21.50 1.60 -8 3 0 20.60 1.60 -8 3 0 17.20 1.70 7 -3 0 13.90 0.90 -7 3 0 12.80 1.40 -7 3 0 11.50 1.20 -7 3 0 9.20 1.00 -7 3 0 11.10 1.10 6 -3 0 36.70 1.80 6 -3 0 34.50 1.40 -6 3 0 34.80 1.70 -6 3 0 33.10 1.70 -6 3 0 33.00 1.80 -6 3 0 32.60 1.90 5 -3 0 24.90 1.30 5 -3 0 23.40 1.10 -5 3 0 24.70 1.50 -5 3 0 26.40 1.30 -5 3 0 23.80 1.40 -5 3 0 22.70 1.30 4 -3 0 133.09 4.00 4 -3 0 136.19 3.90 4 -3 0 133.99 3.90 -4 3 0 133.59 4.00 -4 3 0 129.19 4.00 -4 3 0 130.09 4.10 -4 3 0 126.49 3.90 3 -3 0 394.66 10.90 3 -3 0 385.06 10.80 3 -3 0 401.76 10.70 -3 3 0 381.96 10.80 -3 3 0 384.06 10.90 -3 3 0 377.26 10.90 -3 3 0 365.56 10.80 2 -3 0 415.36 11.70 2 -3 0 416.16 11.70 2 -3 0 423.16 11.60 -2 3 0 412.96 11.70 -2 3 0 403.46 11.70 -2 3 0 422.56 11.70 -2 3 0 430.76 11.70 1 -3 0 786.52 22.60 1 -3 0 795.52 22.50 1 -3 0 792.82 22.50 -1 3 0 809.72 22.50 -1 3 0 835.22 22.60 -1 3 0 813.62 22.60 -1 3 0 862.01 22.50 0 -3 0 83.49 2.70 0 -3 0 85.99 2.60 0 -3 0 86.99 2.70 0 3 0 88.69 2.70 0 3 0 89.29 2.70 0 3 0 86.99 2.60 0 3 0 87.49 2.70 -1 -3 0 174.68 5.30 -1 -3 0 193.38 5.20 -1 -3 0 185.48 5.40 1 3 0 181.78 5.20 1 3 0 176.98 5.30 1 3 0 180.98 5.30 1 3 0 171.78 5.30 -2 -3 0 351.26 10.00 -2 -3 0 359.36 10.20 -2 -3 0 362.86 10.10 2 3 0 342.77 10.10 2 3 0 355.16 9.90 2 3 0 339.07 10.10 2 3 0 359.06 10.10 -3 -3 0 110.29 3.70 -3 -3 0 109.59 3.60 -3 -3 0 112.19 3.70 -3 -3 0 111.69 3.80 3 3 0 111.99 3.30 3 3 0 110.09 3.70 3 3 0 118.49 3.70 -4 -3 0 118.69 4.00 -4 -3 0 116.89 4.10 -4 -3 0 115.89 4.00 4 3 0 125.89 4.00 4 3 0 116.79 3.40 4 3 0 117.09 3.40 -5 -3 0 0.20 1.00 -5 -3 0 0.60 1.00 -5 -3 0 0.80 0.90 5 3 0 1.40 1.00 -6 -3 0 45.30 2.80 -6 -3 0 41.80 2.60 -7 -3 0 2.60 1.60 -7 -3 0 3.20 1.50 -10 4 0 1.60 1.80 -10 4 0 0.20 1.40 -9 4 0 2.40 1.00 -9 4 0 3.30 1.20 -9 4 0 1.10 1.50 -8 4 0 10.80 1.60 -8 4 0 9.10 1.30 -8 4 0 10.90 1.20 7 -4 0 0.70 0.70 -7 4 0 0.60 0.80 -7 4 0 2.20 0.90 -7 4 0 1.00 0.90 -7 4 0 1.70 1.00 6 -4 0 15.40 1.00 -6 4 0 14.90 1.20 -6 4 0 15.20 1.10 -6 4 0 13.10 1.00 -6 4 0 12.80 1.30 5 -4 0 2.40 0.50 -5 4 0 1.90 0.80 -5 4 0 2.40 0.70 -5 4 0 2.00 0.60 -5 4 0 2.30 0.60 4 -4 0 154.78 4.50 -4 4 0 153.28 4.70 -4 4 0 156.18 4.60 -4 4 0 151.68 4.60 -4 4 0 148.79 4.70 -4 4 0 154.18 4.70 3 -4 0 574.14 16.30 3 -4 0 580.64 16.30 -3 4 0 557.54 16.30 -3 4 0 582.04 16.40 -3 4 0 609.74 16.30 -3 4 0 602.64 16.40 2 -4 0 5.30 0.60 2 -4 0 5.10 0.50 2 -4 0 6.40 0.50 -2 4 0 3.80 0.60 -2 4 0 4.40 0.50 -2 4 0 4.50 0.50 -2 4 0 4.50 0.50 1 -4 0 241.68 6.80 1 -4 0 236.88 6.70 1 -4 0 228.78 6.80 -1 4 0 238.08 6.90 -1 4 0 245.48 6.90 -1 4 0 234.28 6.70 -1 4 0 233.28 6.90 0 -4 0 61.69 2.00 0 -4 0 63.39 2.20 0 -4 0 68.89 2.20 0 4 0 64.49 2.00 0 4 0 64.29 2.20 0 4 0 58.79 2.20 0 4 0 62.89 2.20 -1 -4 0 672.23 18.70 -1 -4 0 666.33 18.50 -1 -4 0 682.93 18.80 1 4 0 670.73 18.60 1 4 0 657.23 18.70 1 4 0 644.74 18.70 -2 -4 0 97.29 3.40 -2 -4 0 102.59 3.20 -2 -4 0 104.89 3.40 2 4 0 101.49 3.40 2 4 0 100.69 3.40 2 4 0 99.59 3.10 -3 -4 0 161.78 5.10 -3 -4 0 150.08 4.90 -3 -4 0 161.18 5.00 3 4 0 152.88 4.60 3 4 0 156.28 5.00 -4 -4 0 96.19 3.50 -4 -4 0 89.19 3.50 -4 -4 0 101.69 3.70 4 4 0 94.99 3.60 4 4 0 93.89 2.90 -5 -4 0 10.40 1.50 -5 -4 0 11.20 1.50 -5 -4 0 11.50 1.40 -6 -4 0 33.70 2.30 -6 -4 0 29.90 2.10 -6 -4 0 27.80 2.20 -7 -4 0 2.50 1.70 -7 -4 0 0.50 1.50 -7 -4 0 0.40 1.70 -10 5 0 1.50 1.70 -9 5 0 6.30 1.30 -9 5 0 5.50 1.30 -9 5 0 4.70 1.70 -8 5 0 0.10 1.10 -8 5 0 2.50 1.10 -8 5 0 0.90 1.30 -7 5 0 24.50 1.80 -7 5 0 27.40 1.70 -7 5 0 24.20 1.80 -7 5 0 24.50 1.60 6 -5 0 91.19 2.90 -6 5 0 92.79 3.40 -6 5 0 93.29 3.20 -6 5 0 94.89 3.20 -6 5 0 91.19 3.50 5 -5 0 9.70 0.80 5 -5 0 9.40 0.70 -5 5 0 7.90 1.00 -5 5 0 6.70 1.00 -5 5 0 9.70 0.80 -5 5 0 8.10 0.80 4 -5 0 22.50 1.20 -4 5 0 20.50 1.20 -4 5 0 21.30 1.20 -4 5 0 20.50 1.50 -4 5 0 21.60 1.30 -4 5 0 21.00 1.50 3 -5 0 104.19 3.20 -3 5 0 101.79 3.20 -3 5 0 99.09 3.20 -3 5 0 97.69 3.20 -3 5 0 99.79 3.30 2 -5 0 808.32 22.40 -2 5 0 789.12 22.30 -2 5 0 797.52 22.40 -2 5 0 793.92 22.40 -2 5 0 816.12 22.40 1 -5 0 441.36 12.90 1 -5 0 453.15 12.70 -1 5 0 439.56 12.70 -1 5 0 461.05 12.90 -1 5 0 475.25 12.90 -1 5 0 455.35 12.90 0 -5 0 130.49 3.90 0 -5 0 125.29 4.20 0 -5 0 151.68 4.40 0 5 0 126.29 4.20 0 5 0 132.29 4.10 0 5 0 138.39 4.20 0 5 0 128.19 3.90 -1 -5 0 41.70 1.90 -1 -5 0 41.60 1.90 -1 -5 0 38.60 1.60 1 5 0 42.20 2.00 1 5 0 39.60 1.90 1 5 0 40.70 1.70 -2 -5 0 33.80 2.00 -2 -5 0 36.70 1.70 -2 -5 0 36.20 2.00 2 5 0 35.20 1.60 2 5 0 41.70 2.10 2 5 0 39.10 2.00 -3 -5 0 187.48 5.90 -3 -5 0 190.78 6.20 3 5 0 203.88 6.20 3 5 0 189.98 5.70 -4 -5 0 7.10 1.30 -4 -5 0 7.00 1.10 4 5 0 6.20 1.30 4 5 0 8.20 0.70 -5 -5 0 32.10 2.30 -5 -5 0 30.80 2.30 -6 -5 0 6.60 1.50 -6 -5 0 10.40 1.90 -9 6 0 10.40 1.50 -9 6 0 5.00 1.30 -9 6 0 8.00 1.80 -8 6 0 -0.40 1.10 -8 6 0 -1.40 1.30 -8 6 0 0.90 1.30 -7 6 0 0.90 0.90 -7 6 0 0.00 1.20 -7 6 0 1.60 1.10 -7 6 0 1.90 0.80 6 -6 0 0.00 0.60 -6 6 0 -0.70 0.70 -6 6 0 -0.40 0.90 -6 6 0 0.20 0.90 -6 6 0 -0.30 0.80 5 -6 0 5.60 0.70 -5 6 0 4.50 1.00 -5 6 0 6.50 1.10 -5 6 0 5.30 0.80 -5 6 0 4.40 0.80 4 -6 0 207.88 6.40 -4 6 0 219.28 6.60 -4 6 0 223.18 6.40 -4 6 0 212.28 6.50 3 -6 0 7.00 0.80 -3 6 0 6.50 0.90 -3 6 0 6.10 0.70 -3 6 0 6.80 0.90 -3 6 0 4.50 0.80 2 -6 0 52.29 2.10 -2 6 0 51.49 2.20 -2 6 0 52.19 2.20 -2 6 0 49.60 1.80 -2 6 0 49.90 2.10 1 -6 0 3.50 0.80 1 -6 0 3.70 0.50 -1 6 0 2.90 0.80 -1 6 0 4.10 0.50 -1 6 0 3.80 0.80 -1 6 0 4.20 0.90 0 -6 0 55.29 2.40 0 -6 0 59.59 2.00 0 6 0 53.89 2.40 0 6 0 62.29 2.30 0 6 0 56.59 2.40 -1 -6 0 559.24 15.80 -1 -6 0 572.44 16.10 1 6 0 533.05 16.10 1 6 0 555.14 15.90 1 6 0 585.54 16.10 -2 -6 0 1.10 0.90 -2 -6 0 2.50 0.80 2 6 0 0.20 1.00 2 6 0 1.30 0.70 -3 -6 0 49.00 2.70 -3 -6 0 49.70 2.30 3 6 0 49.90 2.70 3 6 0 49.50 2.00 -4 -6 0 3.00 1.10 -4 -6 0 3.10 1.30 -5 -6 0 39.40 2.70 -5 -6 0 37.50 2.60 -9 7 0 -1.00 1.50 -9 7 0 0.60 1.20 -9 7 0 0.70 1.50 -8 7 0 1.30 1.50 -8 7 0 0.50 1.40 -8 7 0 -0.20 1.10 -7 7 0 5.10 1.40 -7 7 0 4.40 1.10 -7 7 0 5.40 1.40 -6 7 0 11.60 1.10 -6 7 0 10.30 1.40 -6 7 0 9.40 1.30 -6 7 0 9.80 1.10 5 -7 0 48.50 2.10 -5 7 0 53.99 2.60 -5 7 0 48.20 2.20 -5 7 0 54.69 2.60 -5 7 0 45.40 2.20 4 -7 0 2.70 0.80 -4 7 0 3.70 0.90 -4 7 0 1.30 1.00 -4 7 0 2.50 0.80 3 -7 0 54.59 2.20 -3 7 0 49.80 2.30 -3 7 0 53.39 2.50 -3 7 0 49.20 2.00 -3 7 0 50.49 2.20 -2 7 0 34.30 2.00 -2 7 0 33.70 1.50 -2 7 0 37.40 2.00 -2 7 0 34.30 1.90 1 -7 0 1.90 0.90 1 -7 0 2.10 0.50 -1 7 0 2.00 0.90 -1 7 0 2.10 1.00 -1 7 0 2.10 0.90 -1 7 0 2.10 0.50 0 -7 0 106.19 3.90 0 -7 0 107.59 3.30 0 7 0 110.69 3.80 0 7 0 106.39 3.90 0 7 0 109.69 4.00 -1 -7 0 7.00 0.80 -1 -7 0 6.00 1.20 1 7 0 6.50 1.30 1 7 0 7.50 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4 64.49 2.90 -1 7 -4 30.70 2.00 -1 7 -4 27.30 2.00 -1 7 -4 32.40 2.00 1 -7 4 34.00 2.00 1 -7 4 30.00 2.00 -2 7 -4 1.50 0.90 -2 7 -4 1.20 1.00 -2 7 -4 2.30 1.00 2 -7 4 2.10 0.90 2 -7 4 3.10 1.00 -3 7 -4 2.10 0.80 -3 7 -4 1.70 1.00 -3 7 -4 1.30 1.00 -3 7 -4 0.30 0.90 3 -7 4 1.20 0.90 3 -7 4 2.00 1.00 -4 7 -4 74.29 3.10 -4 7 -4 76.69 3.10 -4 7 -4 73.79 3.10 -4 7 -4 77.29 3.00 4 -7 4 71.29 3.00 -5 7 -4 41.20 2.40 -5 7 -4 41.30 2.50 -5 7 -4 44.40 2.50 -6 7 -4 10.60 1.40 -6 7 -4 8.70 1.40 -6 7 -4 5.40 1.30 -7 7 -4 2.40 1.40 -7 7 -4 2.80 1.40 -7 7 -4 1.90 1.40 -8 7 -4 0.60 1.50 -8 7 -4 -0.10 1.50 -8 7 -4 -2.30 1.40 -9 7 -4 0.80 1.70 -9 7 -4 0.80 1.60 -9 7 -4 1.00 1.60 -5 -6 4 9.80 1.70 -5 -6 4 13.50 1.90 -4 -6 4 -0.80 1.20 -4 -6 4 -0.10 1.30 3 6 -4 40.50 2.60 3 6 -4 38.50 1.60 -3 -6 4 38.50 2.40 -3 -6 4 40.30 2.50 2 6 -4 159.68 4.90 2 6 -4 158.28 5.30 -2 -6 4 163.98 5.30 -2 -6 4 160.38 5.30 -2 -6 4 164.28 5.40 1 6 -4 11.10 1.20 1 6 -4 10.60 0.90 -1 -6 4 8.40 1.20 -1 -6 4 11.90 1.30 -1 -6 4 11.30 1.20 0 6 -4 53.89 2.40 0 6 -4 50.79 2.40 0 6 -4 54.79 2.20 0 -6 4 55.59 2.50 0 -6 4 53.89 2.40 -1 6 -4 17.10 1.30 -1 6 -4 15.00 1.20 -1 6 -4 16.60 1.30 1 -6 4 15.50 1.20 1 -6 4 18.70 1.40 -2 6 -4 494.45 14.10 -2 6 -4 502.95 14.10 2 -6 4 477.85 14.10 2 -6 4 491.05 14.10 -3 6 -4 147.59 4.80 -3 6 -4 145.69 4.80 -3 6 -4 154.38 4.80 -3 6 -4 150.68 4.70 3 -6 4 148.39 4.90 3 -6 4 148.79 4.80 -4 6 -4 12.10 1.20 -4 6 -4 14.30 1.20 -4 6 -4 14.40 1.30 -4 6 -4 15.30 1.20 4 -6 4 13.80 1.30 -5 6 -4 2.10 1.00 -5 6 -4 1.20 0.90 -5 6 -4 -0.50 0.80 -5 6 -4 1.30 1.00 5 -6 4 0.80 0.90 -6 6 -4 5.90 1.20 -6 6 -4 6.30 1.20 -6 6 -4 5.00 1.20 -7 6 -4 11.30 1.50 -7 6 -4 9.80 1.50 -7 6 -4 7.30 1.40 -8 6 -4 4.50 1.50 -8 6 -4 2.80 1.40 -8 6 -4 2.40 1.40 -9 6 -4 0.60 1.50 -9 6 -4 1.50 1.50 -9 6 -4 0.20 1.70 -6 -5 4 2.80 1.60 -6 -5 4 -0.20 1.50 -5 -5 4 28.70 2.20 -5 -5 4 32.70 2.20 -4 -5 4 55.69 2.90 -4 -5 4 55.49 2.90 3 5 -4 126.89 3.80 3 5 -4 127.99 4.30 -3 -5 4 127.99 4.40 -3 -5 4 126.59 4.40 -3 -5 4 124.69 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50.49 2.40 -7 5 -4 4.00 1.30 -7 5 -4 2.50 1.20 -7 5 -4 2.20 1.20 -8 5 -4 9.20 1.70 -8 5 -4 9.70 1.60 -8 5 -4 6.40 1.40 -9 5 -4 -2.00 1.30 -9 5 -4 -0.40 1.60 -9 5 -4 -1.60 1.50 -7 -4 4 1.70 1.50 -7 -4 4 0.70 1.60 -6 -4 4 16.20 1.70 -6 -4 4 18.30 1.90 -5 -4 4 60.99 3.00 -5 -4 4 59.29 2.90 4 4 -4 3.10 0.90 -4 -4 4 2.40 1.10 -4 -4 4 3.60 0.90 -4 -4 4 0.90 1.00 3 4 -4 179.28 5.40 3 4 -4 173.48 5.60 3 4 -4 188.18 5.20 -3 -4 4 177.98 5.70 -3 -4 4 186.48 5.20 -3 -4 4 187.18 5.80 -3 -4 4 182.18 5.70 2 4 -4 35.30 1.50 2 4 -4 39.10 1.50 2 4 -4 39.40 1.80 -2 -4 4 41.20 1.90 -2 -4 4 38.10 1.80 -2 -4 4 38.80 1.90 -2 -4 4 37.80 1.40 1 4 -4 300.97 8.50 1 4 -4 301.77 8.60 1 4 -4 305.87 9.00 1 4 -4 308.17 8.80 1 4 -4 306.17 8.80 -1 -4 4 308.27 8.80 -1 -4 4 282.87 8.80 -1 -4 4 294.77 8.70 -1 -4 4 302.17 8.60 0 4 -4 427.36 12.40 0 4 -4 445.76 12.40 0 4 -4 432.66 12.40 0 4 -4 431.26 12.30 0 -4 4 443.46 12.40 0 -4 4 435.36 12.30 0 -4 4 432.46 12.50 -1 4 -4 196.28 5.80 -1 4 -4 195.48 5.70 -1 4 -4 200.48 5.80 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3.40 -5 -3 4 88.59 3.50 4 3 -4 102.59 3.30 4 3 -4 96.39 3.40 -4 -3 4 105.69 3.80 -4 -3 4 105.89 3.40 -4 -3 4 105.49 3.50 -4 -3 4 101.39 3.60 3 3 -4 203.08 5.90 -3 -3 4 209.48 6.30 -3 -3 4 208.08 6.20 -3 -3 4 203.58 6.20 -3 -3 4 203.28 5.80 2 3 -4 3.70 0.50 2 3 -4 3.70 0.60 2 3 -4 4.10 0.70 2 3 -4 3.60 0.40 -2 -3 4 3.80 0.40 -2 -3 4 2.10 0.60 -2 -3 4 2.70 0.60 -2 -3 4 2.80 0.70 1 3 -4 230.28 6.70 1 3 -4 226.78 6.40 1 3 -4 229.48 6.50 1 3 -4 227.88 6.70 1 3 -4 240.48 6.60 -1 -3 4 223.38 6.70 -1 -3 4 225.18 6.60 -1 -3 4 213.58 6.60 -1 -3 4 230.98 6.50 0 3 -4 5.80 0.70 0 3 -4 6.40 0.60 0 3 -4 8.50 0.60 0 3 -4 8.20 0.70 0 -3 4 8.00 0.70 0 -3 4 7.60 0.80 0 -3 4 6.30 0.50 0 -3 4 5.80 0.60 -1 3 -4 247.78 6.90 -1 3 -4 241.88 7.10 -1 3 -4 236.98 7.20 -1 3 -4 249.38 7.10 -1 3 -4 261.57 7.10 1 -3 4 238.68 7.10 1 -3 4 247.38 7.20 1 -3 4 237.58 7.00 1 -3 4 245.38 7.10 -2 3 -4 347.27 9.90 -2 3 -4 341.97 9.70 -2 3 -4 353.06 9.80 -2 3 -4 332.07 9.90 2 -3 4 342.17 9.90 2 -3 4 357.96 9.90 2 -3 4 333.07 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52.99 2.00 -1 -4 5 53.89 2.30 -1 -4 5 55.69 2.20 -1 -4 5 52.49 2.10 -1 -4 5 52.39 1.90 0 4 -5 154.08 4.80 0 4 -5 158.28 4.70 0 -4 5 153.88 4.80 0 -4 5 146.69 4.80 0 -4 5 163.48 4.90 0 -4 5 155.68 4.70 -1 4 -5 0.00 0.60 -1 4 -5 -0.70 0.50 -1 4 -5 -0.50 0.60 -1 4 -5 0.80 0.40 1 -4 5 0.20 0.60 1 -4 5 0.40 0.70 1 -4 5 -0.30 0.50 -2 4 -5 411.96 11.80 -2 4 -5 401.66 11.60 -2 4 -5 420.46 11.80 -2 4 -5 423.76 11.80 2 -4 5 406.26 11.80 2 -4 5 405.26 11.70 2 -4 5 406.06 11.80 -3 4 -5 159.88 5.10 -3 4 -5 173.18 5.20 -3 4 -5 168.58 5.20 -3 4 -5 166.48 5.00 3 -4 5 163.08 5.20 3 -4 5 172.38 5.30 -4 4 -5 0.40 0.80 -4 4 -5 -0.30 0.80 -4 4 -5 0.60 0.70 -4 4 -5 1.50 0.80 4 -4 5 0.40 0.80 -5 4 -5 3.30 1.00 -5 4 -5 2.90 1.00 -5 4 -5 1.70 0.80 -5 4 -5 2.60 1.00 5 -4 5 2.00 0.90 -6 4 -5 70.79 2.90 -6 4 -5 67.59 3.00 -6 4 -5 64.89 3.00 -6 4 -5 68.69 2.90 6 -4 5 60.39 2.60 -7 4 -5 19.00 1.80 -7 4 -5 22.20 1.70 -7 4 -5 19.00 1.80 -8 4 -5 6.00 1.50 -8 4 -5 6.30 1.60 -8 4 -5 5.70 1.40 -9 4 -5 0.10 1.30 -9 4 -5 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-0.60 1.60 1 -7 13 0.10 1.60 1 -7 13 0.60 1.90 -2 7 -13 11.50 2.00 2 -7 13 12.40 2.30 -3 7 -13 23.80 2.40 3 -7 13 20.00 2.50 -1 -6 13 5.30 1.70 -1 -6 13 6.80 2.10 0 -6 13 8.60 1.80 0 -6 13 6.70 2.00 -1 6 -13 0.00 1.50 1 -6 13 -0.60 1.70 1 -6 13 0.40 1.60 -2 6 -13 -0.30 1.60 2 -6 13 1.00 1.60 2 -6 13 -0.40 1.80 -3 6 -13 14.00 2.10 3 -6 13 13.00 2.20 -4 6 -13 7.30 1.90 4 -6 13 11.70 2.10 -3 -5 13 24.00 2.20 -3 -5 13 25.40 2.70 -2 -5 13 3.00 1.90 -2 -5 13 0.80 1.50 -1 -5 13 -0.30 1.80 -1 -5 13 0.80 1.40 0 -5 13 9.50 1.70 0 -5 13 8.40 2.00 1 -5 13 8.00 1.90 1 -5 13 9.80 1.70 2 -5 13 10.40 1.70 2 -5 13 11.60 2.00 3 -5 13 1.70 1.50 3 -5 13 0.10 1.70 4 -5 13 1.80 1.80 -5 5 -13 -0.60 1.30 5 -5 13 1.70 1.90 -4 -4 13 1.00 1.40 -4 -4 13 -0.90 1.80 -3 -4 13 2.40 1.80 -3 -4 13 1.60 1.30 -2 -4 13 35.80 2.70 -2 -4 13 39.10 2.90 -1 -4 13 76.79 3.50 -1 -4 13 73.69 4.00 0 -4 13 -0.30 1.60 0 -4 13 0.50 1.40 1 -4 13 12.40 1.70 1 -4 13 14.50 2.00 2 -4 13 1.70 1.60 2 -4 13 3.40 1.40 -3 4 -13 6.80 1.20 3 -4 13 7.30 1.80 3 -4 13 8.20 1.70 -4 4 -13 5.50 1.30 4 -4 13 5.80 1.70 4 -4 13 6.50 1.80 -5 4 -13 3.60 1.40 -4 -3 13 22.50 2.40 -4 -3 13 20.70 1.80 -3 -3 13 -0.30 1.70 -3 -3 13 0.10 1.20 -2 -3 13 20.30 1.80 -2 -3 13 22.00 2.20 -1 -3 13 15.30 2.00 -1 -3 13 17.20 1.70 0 -3 13 2.50 1.30 0 -3 13 1.90 1.60 1 -3 13 16.70 2.10 1 -3 13 17.50 1.80 -2 3 -13 5.50 1.00 2 -3 13 6.90 1.50 2 -3 13 8.20 1.70 -3 3 -13 8.10 1.20 3 -3 13 9.30 1.70 3 -3 13 7.10 1.70 -4 3 -13 -0.30 1.20 4 -3 13 -0.90 1.60 4 -3 13 0.70 1.60 -5 3 -13 2.60 1.40 -5 -2 13 11.90 1.50 -5 -2 13 5.70 1.90 -4 -2 13 66.49 3.80 -4 -2 13 65.99 3.10 -3 -2 13 7.90 1.90 -3 -2 13 9.10 1.40 -2 -2 13 8.20 1.30 -2 -2 13 8.10 1.70 -1 -2 13 3.90 1.60 -1 -2 13 7.40 1.30 0 -2 13 89.89 3.70 0 -2 13 93.39 4.00 1 -2 13 62.09 3.40 1 -2 13 58.49 3.00 2 -2 13 -1.00 1.20 2 -2 13 0.20 1.40 -3 2 -13 3.80 1.10 3 -2 13 6.20 1.70 3 -2 13 7.80 1.60 -4 2 -13 4.70 1.40 4 -2 13 4.20 1.70 4 -2 13 4.30 1.70 -5 2 -13 10.60 1.70 -5 -1 13 6.40 1.90 -5 -1 13 6.30 1.20 -4 -1 13 5.20 1.80 -4 -1 13 3.70 1.10 -3 -1 13 48.50 2.50 -3 -1 13 41.90 3.10 -2 -1 13 108.19 4.00 -2 -1 13 112.19 4.50 -1 -1 13 2.00 1.10 -1 -1 13 -0.30 1.40 0 -1 13 4.50 1.40 0 -1 13 3.20 1.20 1 -1 13 3.00 1.20 1 -1 13 3.30 1.40 2 -1 13 36.60 2.60 2 -1 13 27.40 2.10 -3 1 -13 4.80 1.20 3 -1 13 2.40 1.50 3 -1 13 3.80 1.50 -4 1 -13 11.20 1.60 4 -1 13 14.00 1.90 -5 1 -13 0.00 1.50 -6 0 13 5.90 1.10 -6 0 13 2.70 1.90 -5 0 13 65.79 3.70 -5 0 13 62.99 2.70 -4 0 13 28.20 2.40 -4 0 13 31.70 2.00 -3 0 13 12.60 1.80 -3 0 13 11.30 1.30 -2 0 13 14.90 1.40 -2 0 13 13.40 1.70 -1 0 13 49.70 2.90 -1 0 13 51.19 2.60 0 0 13 88.39 3.50 0 0 13 88.69 3.80 1 0 13 1.20 1.30 1 0 13 0.30 1.20 1 0 13 0.40 1.20 2 0 13 7.90 1.60 2 0 13 8.40 1.60 3 0 13 6.50 1.60 3 0 13 5.70 1.60 -4 0 -13 16.60 1.90 4 0 13 15.30 2.10 -6 1 13 2.40 0.90 -6 1 13 2.30 1.80 -5 1 13 16.10 2.00 -5 1 13 17.50 1.30 -4 1 13 7.80 1.70 -4 1 13 10.20 1.10 -3 1 13 88.19 3.30 -3 1 13 84.59 3.80 -2 1 13 23.50 1.90 -2 1 13 31.20 2.00 -1 1 13 12.80 1.40 -1 1 13 12.80 1.50 0 1 13 9.20 1.40 0 1 13 9.00 1.50 0 1 13 8.40 1.40 1 1 13 13.40 1.50 1 1 13 13.10 1.60 2 1 13 17.90 1.90 2 1 13 19.10 1.70 3 1 13 0.50 1.50 4 1 13 4.10 1.70 -6 2 13 9.90 0.90 -6 2 13 11.60 2.00 -5 2 13 13.80 1.90 -5 2 13 19.00 1.20 -4 2 13 12.30 1.70 -4 2 13 15.50 1.20 -3 2 13 40.20 2.80 -3 2 13 42.10 2.20 -3 2 13 41.90 2.70 -2 2 13 2.40 1.30 -2 2 13 1.70 1.20 -2 2 13 1.00 1.00 -1 2 13 79.09 3.30 -1 2 13 75.89 3.30 0 2 13 32.80 2.50 0 2 13 36.90 2.30 1 2 13 12.40 1.40 1 2 13 15.50 1.70 2 2 13 20.80 2.10 3 2 13 -1.30 1.50 -5 3 13 22.90 2.20 -5 3 13 25.80 1.60 -5 3 13 24.30 2.10 -4 3 13 2.50 1.50 -4 3 13 2.60 1.40 -4 3 13 3.70 0.90 -3 3 13 20.60 1.50 -3 3 13 18.70 1.70 -2 3 13 15.50 1.40 -2 3 13 11.10 1.40 -1 3 13 71.79 3.30 0 3 13 -1.20 1.20 1 3 13 9.80 1.60 2 3 13 1.30 1.50 -5 4 13 12.70 1.00 -4 4 13 62.39 2.60 -3 4 13 26.40 2.00 -2 4 13 1.30 1.10 -1 4 13 2.00 1.30 0 4 13 3.30 1.50 1 4 13 38.10 2.60 -3 5 13 8.50 1.30 -2 5 13 73.99 3.40 -1 5 13 15.50 1.80 0 -6 14 5.90 2.10 1 -6 14 -1.40 2.00 1 -6 14 0.50 1.70 2 -6 14 1.20 2.00 2 -6 14 0.60 1.60 -1 -5 14 0.80 2.10 -1 -5 14 -1.40 1.50 0 -5 14 5.10 1.70 0 -5 14 5.50 2.00 1 -5 14 -0.40 1.50 1 -5 14 2.50 1.80 2 -5 14 8.80 1.80 2 -5 14 8.60 2.00 3 -5 14 0.30 1.50 3 -5 14 1.50 1.90 -3 -4 14 4.50 2.10 -3 -4 14 4.40 1.60 -2 -4 14 0.90 1.50 -2 -4 14 -1.70 1.80 -1 -4 14 32.20 2.40 -1 -4 14 39.30 2.90 0 -4 14 40.00 3.10 0 -4 14 41.50 3.00 1 -4 14 3.40 1.50 1 -4 14 0.40 1.80 2 -4 14 1.70 1.50 2 -4 14 0.50 1.80 3 -4 14 6.60 1.80 3 -4 14 5.00 1.80 4 -4 14 7.90 2.00 -3 -3 14 44.00 2.90 -3 -3 14 45.40 3.20 -2 -3 14 13.70 1.70 -2 -3 14 9.30 2.10 -1 -3 14 -1.90 1.70 -1 -3 14 -0.50 1.30 0 -3 14 2.60 1.70 0 -3 14 1.80 1.40 1 -3 14 12.60 1.90 1 -3 14 10.10 1.60 2 -3 14 19.60 2.00 2 -3 14 22.30 2.30 3 -3 14 5.10 1.80 3 -3 14 1.60 1.50 -4 3 -14 0.20 1.30 4 -3 14 1.80 1.80 4 -3 14 -0.20 1.20 4 -3 14 0.70 1.60 -4 -2 14 7.80 1.40 -4 -2 14 5.60 2.00 -3 -2 14 5.70 1.90 -3 -2 14 6.20 1.40 -2 -2 14 18.40 2.20 -2 -2 14 22.60 1.80 -1 -2 14 42.50 2.70 -1 -2 14 45.00 3.20 0 -2 14 0.30 1.20 0 -2 14 -0.20 1.40 1 -2 14 6.20 1.70 1 -2 14 6.20 1.50 2 -2 14 0.20 1.30 2 -2 14 1.10 1.60 -3 2 -14 5.90 1.30 3 -2 14 9.80 1.90 3 -2 14 6.20 1.60 3 -2 14 8.10 1.40 -4 2 -14 4.00 1.40 4 -2 14 7.20 1.90 4 -2 14 7.40 1.80 -4 -1 14 18.80 2.40 -4 -1 14 22.90 1.80 -3 -1 14 4.90 1.20 -3 -1 14 2.10 1.70 -2 -1 14 15.80 1.50 -2 -1 14 15.70 2.00 -1 -1 14 21.60 1.80 -1 -1 14 22.00 2.20 0 -1 14 1.40 1.20 0 -1 14 1.60 1.50 1 -1 14 17.50 1.90 1 -1 14 16.90 1.80 2 -1 14 1.20 1.50 2 -1 14 1.70 1.40 2 -1 14 -0.30 1.20 3 -1 14 5.90 1.70 3 -1 14 5.00 1.70 -4 1 -14 2.10 1.40 4 -1 14 2.50 1.70 -5 0 14 12.30 1.40 -5 0 14 11.40 2.10 -4 0 14 44.40 3.40 -4 0 14 45.60 2.40 -3 0 14 -0.40 1.00 -3 0 14 0.80 1.60 -2 0 14 25.30 1.80 -2 0 14 22.00 2.10 -1 0 14 1.80 1.50 -1 0 14 5.50 1.30 0 0 14 33.80 2.50 0 0 14 35.30 2.70 1 0 14 24.40 2.00 1 0 14 19.10 1.90 1 0 14 20.20 1.90 2 0 14 3.80 1.50 2 0 14 3.30 1.50 3 0 14 8.60 1.80 -5 1 14 0.90 1.70 -5 1 14 -0.20 0.90 -4 1 14 4.50 1.10 -4 1 14 2.50 1.70 -3 1 14 36.20 2.50 -3 1 14 37.20 2.30 -2 1 14 136.59 4.70 -2 1 14 129.99 5.00 -1 1 14 12.40 1.50 -1 1 14 15.10 1.80 -1 1 14 11.60 1.60 0 1 14 10.60 1.60 0 1 14 10.90 1.50 0 1 14 10.70 1.70 1 1 14 2.50 1.30 1 1 14 1.80 1.40 2 1 14 5.40 1.60 2 1 14 2.20 1.40 3 1 14 4.80 1.80 -5 2 14 64.29 2.60 -5 2 14 63.49 3.70 -4 2 14 21.10 2.00 -4 2 14 22.00 1.50 -4 2 14 19.70 2.20 -3 2 14 -0.90 1.40 -3 2 14 0.20 1.00 -3 2 14 0.90 1.40 -2 2 14 0.90 1.10 -2 2 14 1.10 1.50 -2 2 14 -0.30 1.30 -1 2 14 18.40 1.70 -1 2 14 20.00 1.70 0 2 14 54.99 3.00 0 2 14 58.09 3.20 1 2 14 9.40 1.70 2 2 14 14.60 1.90 -4 3 14 0.80 1.00 -4 3 14 -1.30 1.50 -3 3 14 65.89 2.90 -2 3 14 14.80 1.50 -1 3 14 6.60 1.40 0 3 14 2.70 1.40 -2 4 14 2.90 1.30 -1 -4 15 2.20 1.60 -1 -4 15 -0.30 1.90 0 -4 15 -0.60 1.80 0 -4 15 2.60 1.50 1 -4 15 0.80 1.40 1 -4 15 -0.90 1.70 2 -4 15 0.00 1.80 2 -4 15 -0.60 1.50 -2 -3 15 21.70 2.50 -2 -3 15 20.60 2.00 -1 -3 15 0.20 1.80 -1 -3 15 -1.10 1.30 0 -3 15 5.70 1.50 0 -3 15 9.10 2.00 1 -3 15 1.20 1.70 1 -3 15 0.10 1.40 2 -3 15 22.00 2.40 2 -3 15 16.80 2.00 3 -3 15 2.20 1.60 -3 -2 15 6.70 2.10 -3 -2 15 7.50 1.50 -2 -2 15 -0.70 1.30 -2 -2 15 0.40 1.80 -1 -2 15 27.10 2.10 -1 -2 15 29.30 2.60 0 -2 15 16.80 2.10 0 -2 15 17.40 1.80 1 -2 15 0.50 1.40 1 -2 15 1.60 1.60 2 -2 15 0.90 1.60 2 -2 15 -0.60 1.40 3 -2 15 1.80 1.30 3 -2 15 3.80 1.70 3 -2 15 2.30 1.80 -3 -1 15 74.19 4.10 -3 -1 15 75.79 3.40 -2 -1 15 7.10 1.40 -2 -1 15 6.20 1.90 -1 -1 15 9.00 1.90 -1 -1 15 8.20 1.50 0 -1 15 1.90 1.60 0 -1 15 1.00 1.30 1 -1 15 21.60 2.00 1 -1 15 20.30 2.10 2 -1 15 17.60 2.00 2 -1 15 18.10 2.10 2 -1 15 21.40 2.00 -3 0 15 -0.60 1.60 -3 0 15 0.80 1.20 -2 0 15 7.60 1.40 -2 0 15 7.80 1.80 -1 0 15 57.29 3.20 -1 0 15 51.99 2.90 0 0 15 19.80 1.90 0 0 15 21.70 2.10 0 0 15 22.20 2.00 1 0 15 0.90 1.50 1 0 15 0.80 1.50 1 0 15 0.00 1.40 2 0 15 3.10 1.60 2 0 15 -0.20 1.50 -3 1 15 3.10 1.70 -3 1 15 5.50 1.30 -2 1 15 17.50 2.10 -2 1 15 16.90 2.00 -2 1 15 19.20 1.70 -1 1 15 1.00 1.60 -1 1 15 3.30 1.50 -1 1 15 3.00 1.30 0 1 15 13.10 1.70 0 1 15 8.50 1.60 1 1 15 25.10 2.20 1 1 15 25.90 2.10 -3 2 15 4.70 1.20 -3 2 15 4.60 1.60 -3 2 15 5.30 1.60 -2 2 15 9.00 1.70 -2 2 15 11.30 1.50 -2 2 15 10.70 1.70 -1 2 15 5.00 1.40 0 2 15 12.00 1.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 88429 _shelx_res_file ; TITL NEW-7 in P-1 shelx.res created by SHELXL-2018/3 at 11:52:00 on 27-Mar-2019 CELL 0.71073 8.0599 8.6086 12.7608 96.548 92.518 111.065 ZERR 2.00 0.0003 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N F S BR UNIT 32 30 6 2 2 2 MERG 2 OMIT 0 0 1 OMIT -3 0 5 OMIT -1 4 3 OMIT 0 1 0 OMIT -2 7 5 OMIT -2 -1 12 OMIT 7 -5 3 HTAB N3 Br1 EQIV $1 -x+1, -y, -z+1 HTAB N3 Br1_$1 HTAB N3 Br1 HTAB N3 Br1_$1 EQIV $2 x+1, y+1, z HTAB C4 Br1_$2 HTAB N3 Br1 HTAB N3 Br1_$1 HTAB C4 Br1_$2 FMAP 2 PLAN 3 SIZE 0.090 0.120 0.160 ACTA BOND $H CONF L.S. 13 WGHT 0.037600 0.222800 FVAR 0.59581 0.50341 BR1 6 0.288365 -0.068461 0.650928 11.00000 0.08423 0.05494 = 0.05450 -0.00748 0.02403 -0.00131 S1 5 0.505353 0.406408 0.725106 11.00000 0.09113 0.06814 = 0.04191 0.01260 0.02027 0.04010 F1 4 1.165233 0.688871 0.071974 11.00000 0.10026 0.12869 = 0.07455 0.03747 0.04391 0.03749 N1 3 0.767691 0.528828 0.482907 11.00000 0.05876 0.04841 = 0.04278 0.00670 0.00935 0.01536 C1 1 0.749076 0.676776 0.664530 11.00000 0.10145 0.05176 = 0.04483 -0.00096 -0.00052 0.02567 AFIX 23 H1A 2 0.765957 0.780305 0.635640 11.00000 -1.20000 H1B 2 0.859205 0.688530 0.704392 11.00000 -1.20000 AFIX 0 N2 3 0.698075 0.534244 0.579508 11.00000 0.07064 0.04940 = 0.03851 0.00316 0.00884 0.01832 C2 1 0.597409 0.638065 0.734314 11.00000 0.14508 0.07591 = 0.04216 0.01170 0.01571 0.06521 AFIX 13 H2A 2 0.506784 0.680819 0.710523 11.00000 -1.20000 AFIX 0 N3 3 0.538928 0.246798 0.540769 11.00000 0.06964 0.04783 = 0.04924 0.00875 0.01991 0.01623 AFIX 3 H3A 2 0.472588 0.153018 0.566419 11.00000 -1.20000 H3B 2 0.598218 0.240158 0.483319 11.00000 -1.20000 AFIX 0 C3 1 0.585108 0.388070 0.603336 11.00000 0.05929 0.05131 = 0.03998 0.00793 0.00785 0.02403 C4 1 0.896223 0.658837 0.464677 11.00000 0.06426 0.05164 = 0.04918 0.00439 0.00161 0.01085 AFIX 43 H4A 2 0.943400 0.751707 0.516854 11.00000 -1.20000 AFIX 0 C5 1 0.969217 0.661887 0.362037 11.00000 0.05037 0.05141 = 0.05347 0.01393 0.00277 0.01186 C6 1 1.098014 0.809240 0.340474 11.00000 0.07334 0.05579 = 0.06626 0.01588 0.00529 0.00736 AFIX 43 H6A 2 1.139096 0.902914 0.392330 11.00000 -1.20000 AFIX 0 C7 1 1.166033 0.818754 0.243132 11.00000 0.07076 0.06922 = 0.08451 0.03617 0.01773 0.01012 AFIX 43 H7A 2 1.254083 0.916970 0.229104 11.00000 -1.20000 AFIX 0 C8 1 1.101138 0.681007 0.168266 11.00000 0.05853 0.08906 = 0.06166 0.03030 0.01957 0.03112 C9 1 0.975586 0.531357 0.186181 11.00000 0.05748 0.07319 = 0.06358 0.00491 0.01410 0.02043 AFIX 43 H9A 2 0.935350 0.438646 0.133610 11.00000 -1.20000 AFIX 0 C10 1 0.911483 0.522853 0.283801 11.00000 0.05146 0.05603 = 0.06268 0.01027 0.01478 0.00922 AFIX 43 H10A 2 0.827792 0.422230 0.298028 11.00000 -1.20000 AFIX 0 PART 1 C11 1 0.689256 0.728926 0.850530 21.00000 0.05214 0.04261 = 0.04256 0.01219 0.01520 0.01823 C12 1 0.557459 0.698308 0.919731 21.00000 0.05965 0.08398 = 0.05924 0.00528 0.01438 0.02147 AFIX 43 H12A 2 0.439229 0.635805 0.894732 21.00000 -1.20000 AFIX 0 C13 1 0.601874 0.761136 1.026915 21.00000 0.08390 0.10056 = 0.04527 0.00891 0.01843 0.04182 AFIX 43 H13A 2 0.513251 0.739287 1.073481 21.00000 -1.20000 AFIX 0 C14 1 0.774744 0.854558 1.063903 21.00000 0.09965 0.08267 = 0.04157 0.00051 0.00571 0.03825 AFIX 43 H14A 2 0.804349 0.898834 1.135130 21.00000 -1.20000 AFIX 0 C15 1 0.904101 0.882195 0.994577 21.00000 0.08548 0.09607 = 0.05525 0.00109 0.00336 0.02866 AFIX 43 H15A 2 1.022734 0.943608 1.019215 21.00000 -1.20000 AFIX 0 C16 1 0.860035 0.820070 0.889265 21.00000 0.06570 0.07695 = 0.04904 0.00303 0.01105 0.01954 AFIX 43 H16A 2 0.949586 0.841027 0.843322 21.00000 -1.20000 AFIX 0 PART 2 C11' 1 0.598234 0.700784 0.849435 -21.00000 0.05074 0.05310 = 0.03557 0.00749 0.01574 0.00862 C12' 1 0.516762 0.813736 0.880535 -21.00000 0.06566 0.05839 = 0.06545 0.02044 0.00949 0.01924 AFIX 43 H12B 2 0.447047 0.841350 0.831371 -21.00000 -1.20000 AFIX 0 C13' 1 0.540843 0.885220 0.986452 -21.00000 0.09225 0.05694 = 0.08343 0.00591 0.04111 0.03061 AFIX 43 H13B 2 0.488252 0.962201 1.007970 -21.00000 -1.20000 AFIX 0 C14' 1 0.638991 0.843663 1.057046 -21.00000 0.09462 0.07299 = 0.04156 -0.00402 0.01296 0.00195 AFIX 43 H14B 2 0.655646 0.893516 1.127240 -21.00000 -1.20000 AFIX 0 C15' 1 0.713317 0.732136 1.028606 -21.00000 0.08651 0.11081 = 0.05470 0.01192 -0.01100 0.03689 AFIX 43 H15B 2 0.779040 0.702274 1.078940 -21.00000 -1.20000 AFIX 0 C16' 1 0.692297 0.659829 0.922643 -21.00000 0.08413 0.09622 = 0.07168 0.00167 0.00819 0.05292 AFIX 43 H16B 2 0.744737 0.582013 0.902974 -21.00000 -1.20000 AFIX 0 HKLF 4 REM NEW-7 in P-1 REM wR2 = 0.0769, GooF = S = 1.035, Restrained GooF = 1.035 for all data REM R1 = 0.0285 for 2672 Fo > 4sig(Fo) and 0.0396 for all 3321 data REM 254 parameters refined using 0 restraints END WGHT 0.0376 0.2228 REM Highest difference peak 0.374, deepest hole -0.482, 1-sigma level 0.040 Q1 1 0.7083 0.5975 0.7756 11.00000 0.05 0.37 Q2 1 0.4023 -0.0661 0.6737 11.00000 0.05 0.35 Q3 1 0.5656 0.3927 0.6769 11.00000 0.05 0.24 ; _shelx_res_checksum 15185 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.28837(4) -0.06846(3) 0.65093(2) 0.07274(12) Uani d 1 . . S S1 0.50535(9) 0.40641(8) 0.72511(4) 0.06317(17) Uani d 1 . . F F1 1.1652(2) 0.6889(3) 0.07197(13) 0.0994(6) Uani d 1 . . N N1 0.7677(2) 0.5288(2) 0.48291(13) 0.0510(4) Uani d 1 . . C C1 0.7491(4) 0.6768(3) 0.66453(19) 0.0676(7) Uani d 1 . . H H1A 0.765957 0.780305 0.635640 0.081 Uiso calc 1 . . H H1B 0.859205 0.688530 0.704392 0.081 Uiso calc 1 . . N N2 0.6981(3) 0.5342(2) 0.57951(13) 0.0540(4) Uani d 1 . . C C2 0.5974(5) 0.6381(4) 0.73431(19) 0.0803(9) Uani d 1 . . H H2A 0.506784 0.680819 0.710523 0.096 Uiso calc 1 A 1 N N3 0.5389(3) 0.2468(2) 0.54077(14) 0.0564(5) Uani d 1 . . H H3A 0.472588 0.153018 0.566419 0.068 Uiso d 1 . . H H3B 0.598218 0.240158 0.483319 0.068 Uiso d 1 . . C C3 0.5851(3) 0.3881(3) 0.60334(16) 0.0489(5) Uani d 1 . . C C4 0.8962(3) 0.6588(3) 0.46468(18) 0.0583(6) Uani d 1 . . H H4A 0.943400 0.751707 0.516854 0.070 Uiso calc 1 . . C C5 0.9692(3) 0.6619(3) 0.36204(18) 0.0532(5) Uani d 1 . . C C6 1.0980(3) 0.8092(3) 0.3405(2) 0.0691(7) Uani d 1 . . H H6A 1.139096 0.902914 0.392330 0.083 Uiso calc 1 . . C C7 1.1660(4) 0.8188(4) 0.2431(2) 0.0767(8) Uani d 1 . . H H7A 1.254083 0.916970 0.229104 0.092 Uiso calc 1 . . C C8 1.1011(3) 0.6810(4) 0.1683(2) 0.0665(7) Uani d 1 . . C C9 0.9756(3) 0.5314(3) 0.1862(2) 0.0659(6) Uani d 1 . . H H9A 0.935350 0.438646 0.133610 0.079 Uiso calc 1 . . C C10 0.9115(3) 0.5229(3) 0.28380(19) 0.0592(6) Uani d 1 . . H H10A 0.827792 0.422230 0.298028 0.071 Uiso calc 1 . . C C11 0.6893(9) 0.7289(7) 0.8505(5) 0.0447(13) Uani d 0.503(4) B 1 C C12 0.5575(7) 0.6983(7) 0.9197(5) 0.0691(15) Uani d 0.503(4) B 1 H H12A 0.439229 0.635805 0.894732 0.083 Uiso calc 0.503(4) B 1 C C13 0.6019(12) 0.7611(13) 1.0269(6) 0.074(2) Uani d 0.503(4) B 1 H H13A 0.513251 0.739287 1.073481 0.089 Uiso calc 0.503(4) B 1 C C14 0.7747(12) 0.8546(10) 1.0639(5) 0.0740(16) Uani d 0.503(4) B 1 H H14A 0.804349 0.898834 1.135130 0.089 Uiso calc 0.503(4) B 1 C C15 0.9041(8) 0.8822(8) 0.9946(4) 0.0811(17) Uani d 0.503(4) B 1 H H15A 1.022734 0.943608 1.019215 0.097 Uiso calc 0.503(4) B 1 C C16 0.8600(7) 0.8201(7) 0.8893(4) 0.0660(14) Uani d 0.503(4) B 1 H H16A 0.949586 0.841027 0.843322 0.079 Uiso calc 0.503(4) B 1 C C11' 0.5982(9) 0.7008(8) 0.8494(5) 0.0489(14) Uani d 0.497(4) B 2 C C12' 0.5168(7) 0.8137(6) 0.8805(4) 0.0631(13) Uani d 0.497(4) B 2 H H12B 0.447047 0.841350 0.831371 0.076 Uiso calc 0.497(4) B 2 C C13' 0.5408(8) 0.8852(7) 0.9865(5) 0.0759(18) Uani d 0.497(4) B 2 H H13B 0.488252 0.962201 1.007970 0.091 Uiso calc 0.497(4) B 2 C C14' 0.6390(15) 0.8437(12) 1.0570(7) 0.079(3) Uani d 0.497(4) B 2 H H14B 0.655646 0.893516 1.127240 0.094 Uiso calc 0.497(4) B 2 C C15' 0.7133(14) 0.7321(12) 1.0286(5) 0.0843(19) Uani d 0.497(4) B 2 H H15B 0.779040 0.702274 1.078940 0.101 Uiso calc 0.497(4) B 2 C C16' 0.6923(8) 0.6598(8) 0.9226(5) 0.0793(17) Uani d 0.497(4) B 2 H H16B 0.744737 0.582013 0.902974 0.095 Uiso calc 0.497(4) B 2 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 0.0842(2) 0.05494(16) 0.05450(16) -0.00131(12) 0.02403(12) -0.00748(11) S1 0.0911(4) 0.0681(4) 0.0419(3) 0.0401(3) 0.0203(3) 0.0126(3) F1 0.1003(12) 0.1287(15) 0.0746(10) 0.0375(11) 0.0439(9) 0.0375(10) N1 0.0588(10) 0.0484(10) 0.0428(9) 0.0154(9) 0.0093(8) 0.0067(8) C1 0.1015(19) 0.0518(13) 0.0448(12) 0.0257(13) -0.0005(12) -0.0010(10) N2 0.0706(12) 0.0494(10) 0.0385(9) 0.0183(9) 0.0088(8) 0.0032(8) C2 0.145(3) 0.0759(18) 0.0422(13) 0.0652(19) 0.0157(15) 0.0117(12) N3 0.0696(11) 0.0478(10) 0.0492(10) 0.0162(9) 0.0199(9) 0.0087(8) C3 0.0593(12) 0.0513(12) 0.0400(10) 0.0240(10) 0.0079(9) 0.0079(9) C4 0.0643(14) 0.0516(13) 0.0492(12) 0.0108(11) 0.0016(10) 0.0044(10) C5 0.0504(12) 0.0514(12) 0.0535(12) 0.0119(10) 0.0028(10) 0.0139(10) C6 0.0733(16) 0.0558(14) 0.0663(15) 0.0074(12) 0.0053(13) 0.0159(12) C7 0.0708(16) 0.0692(17) 0.0845(19) 0.0101(13) 0.0177(14) 0.0362(16) C8 0.0585(14) 0.0891(19) 0.0617(15) 0.0311(14) 0.0196(12) 0.0303(14) C9 0.0575(14) 0.0732(16) 0.0636(15) 0.0204(12) 0.0141(11) 0.0049(12) C10 0.0515(12) 0.0560(13) 0.0627(14) 0.0092(10) 0.0148(11) 0.0103(11) C11 0.052(3) 0.043(3) 0.043(3) 0.018(3) 0.015(3) 0.012(2) C12 0.060(3) 0.084(4) 0.059(4) 0.021(3) 0.014(3) 0.005(3) C13 0.084(6) 0.101(6) 0.045(4) 0.042(5) 0.018(4) 0.009(4) C14 0.100(5) 0.083(5) 0.042(3) 0.038(4) 0.006(3) 0.001(3) C15 0.085(4) 0.096(4) 0.055(3) 0.029(3) 0.003(3) 0.001(3) C16 0.066(3) 0.077(3) 0.049(3) 0.020(3) 0.011(2) 0.003(2) C11' 0.051(4) 0.053(3) 0.036(3) 0.009(3) 0.016(3) 0.007(2) C12' 0.066(3) 0.058(3) 0.065(3) 0.019(2) 0.009(2) 0.020(2) C13' 0.092(4) 0.057(3) 0.083(4) 0.031(3) 0.041(3) 0.006(3) C14' 0.095(7) 0.073(5) 0.042(4) 0.002(5) 0.013(4) -0.004(3) C15' 0.087(5) 0.111(7) 0.055(4) 0.037(5) -0.011(3) 0.012(4) C16' 0.084(4) 0.096(4) 0.072(4) 0.053(4) 0.008(3) 0.002(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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 C3 S1 C2 90.65(11) C4 N1 N2 117.98(19) N2 C1 C2 105.8(2) N2 C1 H1A 110.6 C2 C1 H1A 110.6 N2 C1 H1B 110.6 C2 C1 H1B 110.6 H1A C1 H1B 108.7 C3 N2 N1 116.37(17) C3 N2 C1 115.67(18) N1 N2 C1 127.52(19) C11' C2 C1 129.4(4) C1 C2 C11 104.7(3) C11' C2 S1 104.9(3) C1 C2 S1 105.04(17) C11 C2 S1 112.7(2) C1 C2 H2A 111.4 C11 C2 H2A 111.4 S1 C2 H2A 111.4 C3 N3 H3A 117.3 C3 N3 H3B 119.6 H3A N3 H3B 120.5 N3 C3 N2 123.59(19) N3 C3 S1 123.18(17) N2 C3 S1 113.23(16) N1 C4 C5 120.0(2) N1 C4 H4A 120.0 C5 C4 H4A 120.0 C6 C5 C10 118.6(2) C6 C5 C4 119.1(2) C10 C5 C4 122.3(2) C7 C6 C5 120.8(3) C7 C6 H6A 119.6 C5 C6 H6A 119.6 C8 C7 C6 118.3(2) C8 C7 H7A 120.9 C6 C7 H7A 120.9 F1 C8 C7 119.0(2) F1 C8 C9 117.9(3) C7 C8 C9 123.1(2) C10 C9 C8 118.0(3) C10 C9 H9A 121.0 C8 C9 H9A 121.0 C9 C10 C5 121.2(2) C9 C10 H10A 119.4 C5 C10 H10A 119.4 C16 C11 C12 118.7(5) C16 C11 C2 133.2(5) C12 C11 C2 108.2(5) C11 C12 C13 120.0(6) C11 C12 H12A 120.0 C13 C12 H12A 120.0 C14 C13 C12 120.3(7) C14 C13 H13A 119.8 C12 C13 H13A 119.8 C13 C14 C15 119.0(6) C13 C14 H14A 120.5 C15 C14 H14A 120.5 C16 C15 C14 120.5(6) C16 C15 H15A 119.7 C14 C15 H15A 119.7 C11 C16 C15 121.5(5) C11 C16 H16A 119.2 C15 C16 H16A 119.2 C16' C11' C12' 118.8(6) C16' C11' C2 119.7(5) C12' C11' C2 121.2(5) C11' C12' C13' 119.1(5) C11' C12' H12B 120.4 C13' C12' H12B 120.4 C14' C13' C12' 120.3(6) C14' C13' H13B 119.9 C12' C13' H13B 119.9 C15' C14' C13' 121.0(8) C15' C14' H14B 119.5 C13' C14' H14B 119.5 C14' C15' C16' 119.7(8) C14' C15' H15B 120.1 C16' C15' H15B 120.1 C11' C16' C15' 121.0(6) C11' C16' H16B 119.5 C15' C16' H16B 119.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C3 1.720(2) S1 C2 1.848(3) F1 C8 1.353(3) N1 C4 1.276(3) N1 N2 1.380(2) C1 N2 1.465(3) C1 C2 1.506(4) C1 H1A 0.9700 C1 H1B 0.9700 N2 C3 1.339(3) C2 C11' 1.505(6) C2 C11 1.607(7) C2 H2A 0.9800 N3 C3 1.297(3) N3 H3A 0.9001 N3 H3B 0.9000 C4 C5 1.458(3) C4 H4A 0.9300 C5 C6 1.386(3) C5 C10 1.390(3) C6 C7 1.379(4) C6 H6A 0.9300 C7 C8 1.358(4) C7 H7A 0.9300 C8 C9 1.373(4) C9 C10 1.369(3) C9 H9A 0.9300 C10 H10A 0.9300 C11 C16 1.353(8) C11 C12 1.383(7) C12 C13 1.393(10) C12 H12A 0.9300 C13 C14 1.364(14) C13 H13A 0.9300 C14 C15 1.370(9) C14 H14A 0.9300 C15 C16 1.370(7) C15 H15A 0.9300 C16 H16A 0.9300 C11' C16' 1.333(9) C11' C12' 1.389(8) C12' C13' 1.394(8) C12' H12B 0.9300 C13' C14' 1.334(12) C13' H13B 0.9300 C14' C15' 1.329(15) C14' H14B 0.9300 C15' C16' 1.399(9) C15' H15B 0.9300 C16' H16B 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N3 H3A Br1 . 0.90 2.36 3.2557(18) 172.2 yes N3 H3B Br1 2_656 0.90 2.55 3.3552(18) 149.8 yes C4 H4A Br1 1_665 0.93 2.99 3.726(2) 137.2 yes 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 C4 N1 N2 C3 -169.1(2) C4 N1 N2 C1 3.0(3) C2 C1 N2 C3 -26.1(3) C2 C1 N2 N1 161.8(2) N2 C1 C2 C11' 155.8(4) N2 C1 C2 C11 150.2(3) N2 C1 C2 S1 31.4(2) C3 S1 C2 C11' -163.6(3) C3 S1 C2 C1 -24.92(19) C3 S1 C2 C11 -138.3(3) N1 N2 C3 N3 -0.7(3) C1 N2 C3 N3 -173.7(2) N1 N2 C3 S1 179.87(14) C1 N2 C3 S1 6.8(3) C2 S1 C3 N3 -168.1(2) C2 S1 C3 N2 11.35(19) N2 N1 C4 C5 -177.36(19) N1 C4 C5 C6 174.4(2) N1 C4 C5 C10 -4.2(4) C10 C5 C6 C7 0.8(4) C4 C5 C6 C7 -177.9(2) C5 C6 C7 C8 1.2(4) C6 C7 C8 F1 179.3(2) C6 C7 C8 C9 -2.3(4) F1 C8 C9 C10 179.6(2) C7 C8 C9 C10 1.1(4) C8 C9 C10 C5 1.0(4) C6 C5 C10 C9 -2.0(4) C4 C5 C10 C9 176.7(2) C1 C2 C11 C16 -1.1(7) S1 C2 C11 C16 112.5(6) C1 C2 C11 C12 -179.8(4) S1 C2 C11 C12 -66.2(5) C16 C11 C12 C13 0.1(10) C2 C11 C12 C13 178.9(6) C11 C12 C13 C14 0.8(14) C12 C13 C14 C15 -1.5(15) C13 C14 C15 C16 1.4(12) C12 C11 C16 C15 -0.2(9) C2 C11 C16 C15 -178.7(5) C14 C15 C16 C11 -0.6(10) C1 C2 C11' C16' -64.5(7) S1 C2 C11' C16' 59.9(7) C1 C2 C11' C12' 109.3(6) S1 C2 C11' C12' -126.3(5) C16' C11' C12' C13' 2.2(9) C2 C11' C12' C13' -171.6(5) C11' C12' C13' C14' -0.9(9) C12' C13' C14' C15' -1.0(13) C13' C14' C15' C16' 1.5(16) C12' C11' C16' C15' -1.7(11) C2 C11' C16' C15' 172.2(6) C14' C15' C16' C11' -0.2(14) _cod_database_fobs_code 2242911