#------------------------------------------------------------------------------ #$Date: 2020-04-21 02:36:04 +0300 (Tue, 21 Apr 2020) $ #$Revision: 250963 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240347.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_7240347 loop_ _publ_author_name 'Pereira Copetti, Jo\~ao Pedro' 'Salbego, Paulo Roberto dos Santos' 'Orlando, Tain\'ara' 'Rosa, J\'essica Maria Luis' 'Fiss, Gabriela Fehn' 'Gomes de Oliveira, Jo\~ao Paulo' 'de Almeida Vasconcellos, M\'ario Luiz Ara\'ujo' 'Zanatta, Nilo' 'Bonacorso, Helio Gauze' 'Martins, Marcos A. P.' _publ_section_title ; Substituent Effects in the Crystallization Mechanisms of 7-chloro-4-substituted-Quinolines ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00214C _journal_year 2020 _chemical_formula_moiety 'C11 H11 Cl N2 O' _chemical_formula_sum 'C11 H11 Cl N2 O' _chemical_formula_weight 222.67 _chemical_melting_point ? _chemical_name_common aminoquinolina _chemical_name_systematic 2-((7-chloroquinolin-4-yl)amino)ethanol _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-04-10 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.4840(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.5838(2) _cell_length_b 14.8986(7) _cell_length_c 14.9416(7) _cell_measurement_reflns_used 5230 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 21.0715 _cell_measurement_theta_min 2.4115 _cell_volume 1018.51(8) _computing_cell_refinement 'BRUKER SAINT' _computing_data_collection 'BRUKER APEX-III' _computing_data_reduction 'BRUKER SOFTWARE' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker D8 Venture Photon 100 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type AgK\a _diffrn_radiation_wavelength 0.56086 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 14860 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 19.665 _diffrn_reflns_theta_max 21.086 _diffrn_reflns_theta_min 2.410 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_T_max 0.7446 _exptl_absorpt_correction_T_min 0.6687 _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 1.452 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.530 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.160 _exptl_transmission_factor_max none _exptl_transmission_factor_min none _refine_diff_density_max 0.348 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2235 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0341 _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^)+(0.0658P)^2^+0.2462P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.1008 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1898 _reflns_number_total 2235 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00214c2.cif _cod_data_source_block shelx_CCDC2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'none' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'none' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240347 _shelx_shelxl_version_number 2018/3 _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 0.908 _shelx_estimated_absorpt_t_max 0.971 _exptl_absorpt_special_details none _shelx_res_file ; TITL ag_MMV0297_0m_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 21:15:49 on 09-Apr-2020 CELL 0.56086 4.5838 14.8986 14.9416 90.000 93.484 90.000 ZERR 4.00 0.0002 0.0007 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL UNIT 44 44 8 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.160 0.190 0.530 ACTA BOND $H CONF L.S. 15 TEMP 20.00 OMIT 0 0 2 OMIT 0 2 0 WGHT 0.065800 0.246200 FVAR 0.86226 CL1 5 1.084916 0.405009 0.923485 11.00000 0.02178 0.02172 = 0.01846 0.00085 -0.00591 -0.00028 O1 4 -0.026108 0.447079 0.403049 11.00000 0.02085 0.01049 = 0.01572 -0.00110 -0.00024 -0.00102 AFIX 83 H1 2 0.033621 0.409767 0.368203 11.00000 -1.50000 AFIX 0 N51 3 0.071220 0.353928 0.576804 11.00000 0.01698 0.00977 = 0.01503 0.00050 -0.00128 -0.00073 AFIX 43 H51 2 0.119655 0.409570 0.581530 11.00000 -1.20000 AFIX 0 N1 3 0.471932 0.167280 0.756963 11.00000 0.02059 0.01313 = 0.01928 0.00432 0.00227 0.00030 C8 1 0.831508 0.372000 0.838330 11.00000 0.01359 0.01770 = 0.01288 -0.00003 0.00084 0.00122 C9 1 0.753299 0.283799 0.830113 11.00000 0.01495 0.01577 = 0.01467 0.00514 0.00361 0.00361 AFIX 43 H9 2 0.838362 0.241350 0.869170 11.00000 -1.20000 AFIX 0 C10 1 0.542476 0.256978 0.762049 11.00000 0.01458 0.01358 = 0.01354 0.00348 0.00610 0.00201 C5 1 0.415231 0.322655 0.703191 11.00000 0.01264 0.01286 = 0.01269 0.00073 0.00397 0.00187 C4 1 0.201017 0.293716 0.634095 11.00000 0.01360 0.01332 = 0.01240 0.00073 0.00443 0.00226 C52 1 -0.148441 0.327164 0.507277 11.00000 0.01443 0.01398 = 0.01442 -0.00141 0.00098 -0.00152 AFIX 23 H52A 2 -0.313623 0.300096 0.534654 11.00000 -1.20000 H52B 2 -0.066247 0.282915 0.468383 11.00000 -1.20000 AFIX 0 C53 1 -0.250184 0.408235 0.452548 11.00000 0.01512 0.01326 = 0.01722 -0.00247 -0.00204 0.00149 AFIX 23 H53A 2 -0.411136 0.390514 0.411165 11.00000 -1.20000 H53B 2 -0.322756 0.453223 0.492527 11.00000 -1.20000 AFIX 0 C2 1 0.281286 0.143895 0.690948 11.00000 0.02208 0.01076 = 0.02140 0.00141 0.00388 -0.00119 AFIX 43 H2 2 0.235029 0.083268 0.685737 11.00000 -1.20000 AFIX 0 C3 1 0.143470 0.201991 0.628478 11.00000 0.01824 0.01498 = 0.01467 -0.00078 0.00229 -0.00121 AFIX 43 H3 2 0.014301 0.179667 0.583476 11.00000 -1.20000 AFIX 0 C6 1 0.506985 0.412961 0.713409 11.00000 0.01829 0.01286 = 0.01509 0.00282 0.00093 0.00262 AFIX 43 H6 2 0.426774 0.456279 0.674428 11.00000 -1.20000 AFIX 0 C7 1 0.711645 0.438073 0.779534 11.00000 0.01665 0.01172 = 0.01786 0.00017 0.00098 -0.00010 AFIX 43 H7 2 0.770152 0.497660 0.785419 11.00000 -1.20000 AFIX 0 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM ag_MMV0297_0m_a.res in P2(1)/n REM wR2 = 0.1008, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0341 for 1898 Fo > 4sig(Fo) and 0.0434 for all 2235 data REM 136 parameters refined using 0 restraints END WGHT 0.0436 0.5832 REM Highest difference peak 0.348, deepest hole -0.364, 1-sigma level 0.052 Q1 1 0.0253 0.4089 0.6005 11.00000 0.05 0.35 Q2 1 0.2916 0.3121 0.6754 11.00000 0.05 0.30 Q3 1 0.8203 0.4024 0.8018 11.00000 0.05 0.26 Q4 1 -0.1892 0.3691 0.4775 11.00000 0.05 0.24 Q5 1 0.4438 0.2906 0.7376 11.00000 0.05 0.24 Q6 1 0.2196 0.1801 0.6605 11.00000 0.05 0.23 Q7 1 -0.0325 0.3388 0.5419 11.00000 0.05 0.22 Q8 1 0.6393 0.2749 0.8035 11.00000 0.05 0.22 Q9 1 0.6294 0.4173 0.7406 11.00000 0.05 0.22 Q10 1 0.5072 0.2105 0.7628 11.00000 0.05 0.22 Q11 1 -0.0510 0.4203 0.3380 11.00000 0.05 0.22 Q12 1 0.4732 0.3619 0.7049 11.00000 0.05 0.22 Q13 1 0.8343 0.3240 0.8178 11.00000 0.05 0.21 Q14 1 0.7526 0.3311 0.8410 11.00000 0.05 0.20 Q15 1 0.4667 0.1556 0.8024 11.00000 0.05 0.19 Q16 1 0.1605 0.3209 0.6050 11.00000 0.05 0.19 Q17 1 0.2104 0.2442 0.6291 11.00000 0.05 0.18 Q18 1 -0.1206 0.4205 0.4222 11.00000 0.05 0.17 Q19 1 -0.0114 0.4060 0.3164 11.00000 0.05 0.17 Q20 1 0.5891 0.1462 0.7860 11.00000 0.05 0.16 ; _shelx_res_checksum 68662 _shelx_hkl_file ; 1 0 0 -1.10 1.00 1 0 0 -0.20 1.30 -2 0 0 393.36 7.90 2 0 0 407.86 10.20 2 0 0 382.26 11.70 3 0 0 10.70 4.00 3 0 0 -0.40 4.00 4 0 0 106.89 9.40 4 0 0 108.09 9.20 5 0 0 18.60 7.40 5 0 0 0.70 8.30 1 -1 0 3733.33 65.29 -1 -1 0 3766.42 67.19 -1 -1 0 3782.22 65.59 1 1 0 3796.12 65.59 1 1 0 3595.94 66.99 2 -1 0 278.37 8.90 -2 -1 0 280.37 8.10 2 -1 0 279.37 5.90 2 -1 0 270.37 5.90 -2 -1 0 280.67 9.90 2 1 0 292.87 8.00 2 1 0 299.97 10.00 3 -1 0 1.70 4.10 3 -1 0 10.30 4.70 3 1 0 7.00 4.80 3 1 0 7.90 3.30 4 -1 0 97.79 8.80 4 -1 0 102.99 9.60 4 1 0 117.39 11.00 4 1 0 94.19 7.30 5 -1 0 79.09 8.40 5 -1 0 57.89 11.00 5 1 0 78.39 12.60 5 1 0 66.49 9.60 0 -2 0 394.36 8.10 -1 -2 0 1856.41 35.60 1 -2 0 1847.32 34.10 1 -2 0 1812.82 34.10 -1 -2 0 1891.11 33.50 1 2 0 1861.21 33.40 -1 2 0 1864.31 34.40 1 2 0 1823.82 35.40 -2 -2 0 161.88 8.20 2 -2 0 175.18 5.60 2 -2 0 180.38 5.50 2 -2 0 173.58 6.80 -2 -2 0 173.48 4.30 -2 -2 0 177.78 6.20 2 2 0 176.08 5.80 2 2 0 172.88 8.20 3 -2 0 1972.90 40.10 3 2 0 1899.71 37.70 3 2 0 1918.21 41.70 4 -2 0 10.50 5.20 4 -2 0 18.60 6.40 4 2 0 12.60 4.30 4 2 0 6.10 7.40 5 -2 0 36.30 7.80 5 -2 0 31.80 9.90 5 2 0 39.90 10.70 0 -3 0 0.60 1.20 0 -3 0 0.90 0.90 0 -3 0 0.80 1.10 0 3 0 0.70 1.30 0 3 0 1.10 1.00 0 3 0 0.40 1.00 -1 -3 0 792.62 17.80 -1 -3 0 782.12 15.40 1 -3 0 765.42 16.80 1 -3 0 750.82 16.70 1 3 0 785.42 15.30 1 3 0 819.12 17.70 -1 3 0 765.52 17.10 2 -3 0 343.77 9.50 -2 -3 0 339.97 9.30 -2 -3 0 353.56 12.30 2 -3 0 352.96 9.70 2 3 0 350.46 9.00 2 3 0 355.36 12.00 -2 3 0 333.17 10.20 -3 -3 0 196.58 11.90 -3 -3 0 197.08 5.70 -3 -3 0 198.88 8.60 3 -3 0 205.38 6.90 3 -3 0 193.38 9.30 -3 -3 0 199.18 5.20 3 3 0 196.58 7.60 3 3 0 199.18 11.40 4 -3 0 285.07 14.20 4 -3 0 257.67 13.50 4 3 0 299.77 15.90 4 3 0 282.17 11.20 5 -3 0 87.29 12.10 5 -3 0 63.49 8.60 5 3 0 38.90 12.90 5 3 0 55.39 7.80 0 -4 0 4874.61 86.29 0 -4 0 4846.81 86.39 0 -4 0 5009.70 87.69 0 -4 0 4921.41 87.89 0 4 0 4766.22 86.19 0 4 0 4880.11 86.19 1 -4 0 36.00 3.70 -1 -4 0 28.90 2.40 -1 -4 0 39.40 4.00 -1 -4 0 35.10 4.10 -1 4 0 31.80 3.70 1 4 0 33.30 2.70 1 4 0 32.20 3.70 2 -4 0 149.79 7.10 -2 -4 0 145.69 6.20 2 -4 0 163.48 7.30 -2 -4 0 152.88 5.90 -2 -4 0 165.18 9.30 2 4 0 150.38 8.60 -2 4 0 150.28 7.80 2 4 0 151.58 5.60 3 -4 0 308.07 9.80 3 -4 0 318.87 9.90 3 -4 0 315.17 10.90 -3 -4 0 303.97 8.40 -3 -4 0 301.07 8.30 -3 -4 0 312.27 10.50 -3 -4 0 292.47 14.20 3 4 0 314.97 14.20 3 4 0 320.87 9.90 4 -4 0 79.39 8.80 4 -4 0 92.09 5.50 4 4 0 88.89 10.70 4 4 0 84.49 8.00 5 -4 0 56.49 9.50 5 -4 0 49.20 10.30 5 4 0 34.20 11.40 5 4 0 57.59 7.30 0 -5 0 -2.00 2.40 0 -5 0 -2.60 2.60 0 -5 0 -0.10 1.70 0 -5 0 2.30 2.00 0 5 0 1.60 1.60 0 5 0 1.50 1.50 -1 -5 0 1135.59 24.80 1 -5 0 1056.99 24.20 1 -5 0 1090.79 24.40 -1 -5 0 1132.49 23.70 -1 -5 0 1118.49 22.10 -1 -5 0 1149.29 23.70 -1 5 0 1087.29 24.60 1 5 0 1135.79 24.40 1 5 0 1113.69 22.10 2 -5 0 576.54 15.30 -2 -5 0 593.54 13.70 -2 -5 0 549.74 14.10 2 -5 0 572.54 15.50 -2 -5 0 567.84 14.40 -2 -5 0 557.54 17.50 2 5 0 582.44 17.00 2 5 0 586.64 13.20 -2 5 0 568.44 16.20 3 -5 0 52.29 5.50 -3 -5 0 31.60 3.80 -3 -5 0 45.50 7.70 3 -5 0 50.69 5.50 -3 -5 0 45.00 4.50 -3 -5 0 48.00 4.90 3 5 0 51.79 4.60 3 5 0 57.29 8.10 -4 -5 0 74.49 10.80 -4 -5 0 95.19 7.50 -4 -5 0 89.39 6.10 4 -5 0 104.49 9.00 -4 -5 0 94.99 5.40 4 -5 0 84.89 7.10 4 5 0 93.49 11.00 4 5 0 82.89 6.70 5 -5 0 513.45 21.00 5 -5 0 531.45 20.80 5 5 0 522.65 17.00 5 5 0 481.55 24.80 0 -6 0 954.50 22.20 0 -6 0 959.90 20.30 0 -6 0 944.41 20.50 0 -6 0 970.40 22.50 0 6 0 945.51 20.00 0 6 0 967.80 20.30 -1 -6 0 154.08 7.70 -1 -6 0 143.49 8.00 1 -6 0 142.99 4.90 -1 -6 0 162.08 8.30 -1 -6 0 150.08 5.90 1 -6 0 153.88 8.50 1 -6 0 148.49 8.30 1 6 0 153.88 7.60 1 6 0 144.69 5.80 -1 6 0 125.39 8.50 -2 -6 0 93.69 5.50 -2 -6 0 80.79 6.90 2 -6 0 79.89 7.10 -2 -6 0 78.09 7.80 -2 -6 0 76.49 6.60 2 6 0 87.39 8.10 -2 6 0 95.29 8.50 2 6 0 86.09 4.90 -3 -6 0 404.66 17.30 3 -6 0 388.86 13.50 -3 -6 0 395.36 12.60 3 -6 0 424.06 13.80 -3 -6 0 418.36 12.70 3 6 0 424.46 11.90 4 -6 0 83.69 8.00 4 -6 0 98.29 8.70 -4 -6 0 82.59 7.60 -4 -6 0 81.99 11.60 -4 -6 0 85.79 8.00 -4 -6 0 95.39 6.80 4 -6 0 90.39 7.00 4 6 0 76.69 11.10 4 6 0 93.09 7.30 5 -6 0 84.19 11.50 5 -6 0 78.99 7.10 5 -6 0 84.89 6.80 5 -6 0 94.19 10.60 5 6 0 65.89 9.30 5 6 0 85.29 14.20 0 -7 0 61.69 5.20 1 -7 0 168.78 9.60 -1 -7 0 144.19 8.20 -1 -7 0 184.28 9.20 -1 -7 0 164.68 8.80 1 -7 0 151.28 9.30 1 -7 0 167.58 7.80 -1 -7 0 165.48 6.80 1 -7 0 160.38 6.00 1 7 0 188.18 8.50 1 7 0 161.58 6.70 -2 -7 0 1066.59 25.00 2 -7 0 1062.99 26.50 2 -7 0 1059.09 26.40 -2 -7 0 1120.79 28.50 -2 -7 0 1161.48 25.70 -2 -7 0 1088.99 23.50 2 7 0 1097.29 23.10 2 7 0 1106.29 27.40 3 -7 0 84.99 7.80 -3 -7 0 78.59 6.80 -3 -7 0 68.09 6.60 3 -7 0 82.89 7.70 -3 -7 0 77.99 6.70 -3 -7 0 67.79 9.70 3 7 0 80.59 6.50 3 7 0 83.19 9.30 -4 -7 0 839.72 29.90 -4 -7 0 845.72 20.10 -4 -7 0 853.01 20.80 4 -7 0 873.01 22.20 4 -7 0 843.12 22.40 4 -7 0 870.91 22.60 -4 -7 0 848.22 22.00 4 7 0 843.92 28.40 4 7 0 821.82 20.70 -5 -7 0 58.39 5.80 -5 -7 0 52.79 4.90 5 -7 0 70.09 6.90 5 -7 0 62.59 6.70 5 -7 0 73.39 10.00 5 7 0 58.19 13.50 0 -8 0 1092.99 26.30 0 -8 0 1080.89 26.10 0 -8 0 1020.00 23.80 0 -8 0 1061.29 23.60 0 8 0 1044.90 22.80 0 8 0 1077.69 23.60 1 -8 0 44.10 6.10 1 -8 0 55.89 6.50 -1 -8 0 58.29 6.40 -1 -8 0 49.10 6.20 1 -8 0 49.70 4.90 1 -8 0 44.00 4.60 -1 -8 0 45.70 4.40 1 8 0 51.09 4.40 1 8 0 55.19 5.60 2 -8 0 11.70 6.00 2 -8 0 18.40 6.20 -2 -8 0 10.80 3.50 -2 -8 0 3.90 5.70 -2 -8 0 11.10 4.60 -2 -8 0 13.00 4.40 2 8 0 18.50 3.50 2 8 0 12.10 5.30 -3 -8 0 334.37 17.70 3 -8 0 311.27 14.40 -3 -8 0 329.87 13.20 -3 -8 0 325.07 12.00 3 -8 0 313.27 13.80 -3 -8 0 334.77 13.40 3 8 0 324.47 16.60 3 8 0 337.27 11.30 4 -8 0 28.60 6.40 -4 -8 0 24.60 6.60 -4 -8 0 14.80 6.50 -4 -8 0 31.10 10.20 4 -8 0 20.90 7.10 4 8 0 18.20 5.30 4 8 0 18.30 10.20 -5 -8 0 6.20 5.60 5 -8 0 6.50 7.20 -5 -8 0 0.20 4.80 5 -8 0 8.90 6.70 5 -8 0 3.10 8.60 5 8 0 -6.00 14.80 5 8 0 2.80 6.40 0 -9 0 18.70 5.70 0 -9 0 13.70 4.40 0 -9 0 0.50 3.50 0 -9 0 15.90 4.60 0 9 0 11.20 3.50 -1 -9 0 84.19 8.10 -1 -9 0 78.19 7.50 -1 -9 0 83.89 8.10 1 -9 0 83.19 8.40 1 -9 0 76.89 8.20 1 -9 0 83.29 5.70 -1 -9 0 96.49 6.50 1 -9 0 80.29 6.70 1 9 0 94.39 6.40 1 9 0 87.79 7.70 2 -9 0 384.26 15.90 -2 -9 0 407.76 17.30 -2 -9 0 434.96 15.60 -2 -9 0 403.56 12.30 2 -9 0 392.06 16.00 2 -9 0 390.26 10.30 -2 -9 0 416.86 15.40 2 9 0 381.86 18.10 2 9 0 419.86 12.30 -3 -9 0 265.17 11.50 -3 -9 0 259.37 13.90 -3 -9 0 262.27 13.60 3 -9 0 279.47 14.30 -3 -9 0 281.77 17.50 3 -9 0 242.28 14.20 3 9 0 261.67 10.90 3 9 0 276.17 16.40 -4 -9 0 68.09 8.20 4 -9 0 75.69 7.90 -4 -9 0 60.49 8.50 4 -9 0 68.89 9.90 4 -9 0 46.40 9.30 4 9 0 65.59 7.10 4 9 0 64.89 12.20 5 -9 0 54.19 9.20 -5 -9 0 58.29 7.30 5 -9 0 62.59 9.50 -5 -9 0 59.09 8.40 5 -9 0 74.39 10.40 5 9 0 56.29 8.00 5 9 0 48.00 14.70 0 -10 0 123.79 8.20 0 -10 0 121.09 11.20 0 -10 0 113.79 11.00 0 -10 0 111.19 9.00 0 10 0 114.99 7.10 -1 -10 0 10.60 3.80 1 -10 0 5.60 6.60 -1 -10 0 6.20 5.90 1 -10 0 20.60 5.60 1 -10 0 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-10 15 117.39 14.00 0 -10 -15 160.08 12.10 0 10 15 145.09 17.00 0 10 -15 148.59 13.00 0 10 -15 128.29 17.20 1 -10 15 19.30 9.40 -1 -10 -15 5.50 10.50 -1 -10 -15 26.40 7.80 1 -10 15 15.60 11.20 -1 10 -15 28.90 14.80 -1 10 -15 31.00 10.30 1 10 15 29.70 13.50 1 -11 -15 -10.60 10.60 1 -11 -15 35.40 14.00 -1 -11 15 0.60 10.70 -1 11 15 27.40 15.20 1 11 -15 -3.50 13.90 1 11 -15 -10.80 12.90 0 -11 -15 67.99 10.40 0 -11 -15 40.20 11.40 0 -11 15 98.19 15.30 0 -11 -15 63.99 14.30 0 -11 15 39.60 10.60 0 11 15 97.59 16.00 0 11 -15 47.80 16.60 0 11 -15 86.69 13.50 1 -11 15 1.40 11.90 -1 -11 -15 -5.20 11.50 1 -11 15 1.80 9.70 -1 -11 -15 3.90 7.80 1 11 15 7.40 14.80 -1 11 -15 10.10 10.40 -1 11 -15 -4.20 9.60 -3 0 16 -13.10 9.00 3 0 -16 1.80 10.20 -2 0 16 246.78 17.70 2 0 -16 269.47 16.80 2 0 -16 191.28 17.70 -1 0 16 -19.60 7.50 1 0 -16 -3.40 6.90 1 0 -16 -3.60 9.00 0 0 16 14.90 8.90 0 0 16 -0.30 7.80 0 0 -16 4.30 9.20 0 0 -16 11.80 6.50 1 0 16 3.30 8.20 -1 0 -16 -3.90 9.00 -1 0 -16 3.30 5.30 1 0 16 12.40 6.40 2 0 16 131.39 12.80 -2 0 -16 139.49 9.50 2 0 16 130.49 10.00 3 -1 -16 17.80 10.40 -3 -1 16 14.80 9.60 3 1 -16 3.70 12.00 -2 -1 16 52.19 11.40 2 -1 -16 66.79 10.80 2 -1 -16 50.89 10.90 2 1 -16 72.79 9.40 -2 1 16 50.89 11.20 2 1 -16 74.59 11.50 1 -1 -16 92.39 11.70 -1 -1 16 75.59 10.50 1 -1 -16 97.19 10.50 1 1 -16 89.89 10.70 -1 1 16 77.39 10.10 1 1 -16 95.39 10.50 0 -1 -16 478.15 17.20 0 -1 -16 458.85 21.40 0 -1 16 424.96 18.10 0 -1 16 453.55 21.00 0 1 16 472.85 17.90 0 1 16 489.15 21.60 0 1 -16 457.75 16.50 0 1 -16 478.65 21.80 1 -1 16 186.98 12.70 -1 -1 -16 177.08 17.00 -1 -1 -16 215.58 10.70 1 -1 16 177.88 16.10 -1 1 -16 223.08 18.10 1 1 16 222.28 12.10 1 1 16 223.68 17.00 -1 1 -16 226.68 11.40 2 -1 16 -0.40 10.70 2 -1 16 -4.80 6.00 -2 -1 -16 7.00 4.50 2 1 16 -7.20 5.80 2 1 16 -12.10 10.70 -2 1 -16 5.80 8.50 3 -2 -16 -9.50 11.80 -3 -2 16 10.00 9.90 3 2 -16 6.10 10.90 2 -2 -16 51.99 10.60 -2 -2 16 51.79 10.90 2 -2 -16 63.29 11.30 2 2 -16 57.69 10.60 2 2 -16 64.09 11.60 -1 -2 16 89.09 10.40 1 -2 -16 93.79 11.90 1 -2 -16 63.49 10.20 1 2 -16 85.59 9.40 1 2 -16 81.69 12.20 -1 2 16 102.99 10.40 0 -2 16 281.37 18.20 0 -2 -16 269.27 18.10 0 -2 -16 290.47 13.10 0 2 -16 282.07 14.00 0 2 16 254.77 18.70 0 2 16 284.27 14.50 0 2 -16 262.47 19.30 -1 -2 -16 50.79 12.00 1 -2 16 57.89 9.80 -1 -2 -16 51.79 6.10 1 -2 16 29.90 7.00 -1 2 -16 27.30 10.50 -1 2 -16 39.00 8.10 1 2 16 33.20 11.20 2 -2 16 26.60 7.30 -2 -2 -16 9.50 4.30 2 -2 16 13.30 10.10 -2 2 -16 14.80 7.20 2 2 16 26.30 10.20 -3 -3 16 61.59 13.70 3 -3 -16 47.10 12.30 3 3 -16 75.59 12.80 2 -3 -16 28.80 10.30 -2 -3 16 13.50 9.70 2 -3 -16 23.80 9.70 2 3 -16 42.80 11.20 2 3 -16 30.80 8.30 1 -3 -16 7.70 7.60 -1 -3 16 -5.30 8.10 1 -3 -16 4.70 9.70 1 3 -16 6.20 7.40 1 3 -16 -1.90 9.50 0 -3 -16 230.38 17.80 0 -3 16 261.47 15.10 0 -3 -16 234.48 13.40 0 -3 16 270.67 17.70 0 3 -16 225.58 13.30 0 3 16 258.87 18.90 0 3 -16 230.18 19.40 1 -3 16 108.99 11.60 1 -3 16 107.99 9.30 -1 3 -16 116.89 11.00 -1 3 -16 71.39 12.90 1 3 16 105.39 13.00 2 -3 16 41.60 7.40 -2 -3 -16 49.80 5.00 2 -3 16 50.09 12.30 2 3 16 51.79 13.20 3 -4 -16 9.80 12.30 -3 -4 16 -9.00 11.80 3 4 -16 -4.70 10.70 -2 -4 16 178.08 14.80 2 -4 -16 155.18 13.50 2 -4 -16 164.28 14.70 2 4 -16 145.19 13.30 2 4 -16 154.78 14.50 -1 -4 16 355.36 18.40 1 -4 -16 325.37 20.10 1 -4 -16 319.97 16.60 1 4 -16 344.17 17.00 1 4 -16 357.16 20.90 0 -4 -16 4.80 6.90 0 -4 -16 -1.10 9.00 0 -4 16 5.40 9.30 0 -4 16 0.20 6.70 0 4 -16 -1.00 7.60 0 4 16 -0.10 10.20 0 4 -16 -5.50 10.10 1 -4 16 21.40 9.80 1 -4 16 10.10 7.90 -1 4 -16 18.80 7.10 1 4 16 15.30 10.90 -1 4 -16 15.60 10.60 2 -4 16 163.28 13.70 -2 -4 -16 158.68 7.20 2 -4 16 151.18 13.70 2 4 16 182.18 17.90 3 -5 -16 41.60 12.00 -3 -5 16 23.80 12.70 3 5 -16 35.30 14.00 2 -5 -16 20.60 10.80 2 -5 -16 20.90 10.60 -2 -5 16 33.50 9.60 2 5 -16 30.80 11.90 2 5 -16 35.40 10.40 1 -5 -16 39.30 11.30 -1 -5 16 55.89 9.00 1 -5 -16 34.00 9.20 1 5 -16 70.29 10.10 1 5 -16 41.90 11.50 0 -5 16 32.70 8.40 0 -5 16 49.50 10.50 0 -5 -16 29.60 10.60 0 -5 -16 30.80 7.90 0 5 16 50.19 11.70 0 5 -16 35.90 12.00 0 5 -16 25.00 8.10 1 -5 16 191.08 17.00 1 -5 16 186.18 14.60 -1 5 -16 188.28 12.90 1 5 16 209.88 17.80 -1 5 -16 206.68 20.20 2 -5 16 5.40 6.50 -2 -5 -16 -3.20 3.20 2 -5 16 -2.80 9.80 2 5 16 3.10 11.90 2 -6 -16 -3.10 11.00 2 -6 -16 25.10 10.60 -2 -6 16 26.20 11.20 2 6 -16 2.40 11.40 -1 -6 16 -0.30 8.90 1 -6 -16 -10.40 9.50 1 -6 -16 -7.50 10.80 1 6 -16 4.20 8.50 1 6 -16 13.00 11.30 0 -6 -16 147.09 10.90 0 -6 -16 141.09 14.10 0 -6 16 156.58 14.10 0 -6 16 137.39 11.80 0 6 -16 125.09 15.10 0 6 -16 165.28 13.70 0 6 16 128.69 15.30 -1 -6 -16 21.00 8.80 1 -6 16 31.20 8.00 1 -6 16 17.40 9.50 1 6 16 22.30 10.80 -1 6 -16 9.70 11.70 -1 6 -16 24.80 7.80 2 -6 16 16.10 10.20 2 -6 16 13.40 7.10 -2 -6 -16 10.20 3.50 2 6 16 35.00 13.40 -2 6 -16 39.00 8.70 -2 -7 16 146.99 15.00 2 -7 -16 132.59 14.80 2 -7 -16 136.69 15.00 2 7 -16 110.89 15.90 -1 -7 16 77.29 10.30 1 -7 -16 90.19 13.50 1 -7 -16 73.99 11.90 -1 7 16 92.69 14.70 1 7 -16 64.79 14.10 1 7 -16 76.69 9.90 0 -7 -16 246.08 13.20 0 -7 16 259.47 17.00 0 -7 16 225.68 19.20 0 -7 -16 223.08 20.00 0 7 -16 228.38 22.50 0 7 16 184.98 17.40 0 7 -16 238.68 15.80 1 -7 16 8.00 9.80 1 -7 16 13.30 8.50 -1 -7 -16 21.40 6.80 -1 -7 -16 23.70 9.90 1 7 16 27.00 12.60 -1 7 -16 42.70 12.90 -1 7 -16 26.80 8.70 -2 -7 -16 11.20 10.80 2 -7 16 10.30 11.30 2 -7 16 13.20 7.80 -2 -7 -16 19.10 3.60 -2 7 -16 13.40 9.40 2 7 16 16.80 12.60 2 -8 -16 41.80 14.00 -2 -8 16 75.39 11.50 2 -8 -16 35.10 12.40 2 8 -16 45.80 14.20 1 -8 -16 540.05 23.30 -1 -8 16 510.95 21.10 1 -8 -16 528.35 25.80 1 8 -16 492.55 22.00 1 8 -16 500.85 27.80 -1 8 16 505.05 32.50 0 -8 16 -0.60 8.50 0 -8 16 0.20 10.10 0 -8 -16 12.50 6.70 0 -8 -16 9.00 10.70 0 8 16 -0.60 11.40 0 8 -16 -5.20 8.90 0 8 -16 16.20 13.50 1 -8 16 246.58 16.30 -1 -8 -16 196.68 12.40 -1 -8 -16 179.78 17.20 1 -8 16 251.07 19.40 -1 8 -16 247.78 18.50 1 8 16 215.68 21.70 -1 8 -16 206.88 18.80 -1 -9 16 84.09 12.60 1 -9 -16 80.19 11.60 1 -9 -16 65.39 14.50 1 9 -16 58.29 15.20 -1 9 16 68.69 14.50 0 -9 16 44.80 11.10 0 -9 16 48.20 12.30 0 -9 -16 13.80 12.50 0 -9 -16 53.49 9.90 0 9 -16 26.50 14.60 0 9 -16 66.19 10.70 0 9 16 23.50 14.40 -1 -9 -16 22.00 11.30 -1 -9 -16 44.20 7.70 1 -9 16 28.00 11.70 1 -9 16 22.70 9.50 1 9 16 33.60 14.10 -1 9 -16 42.60 15.50 -1 9 -16 37.80 10.80 1 -10 -16 -1.30 13.20 -1 -10 16 19.40 11.40 1 -10 -16 10.50 12.00 1 10 -16 -5.30 14.30 -1 10 16 0.80 14.50 0 -10 -16 6.20 9.60 0 -10 -16 15.10 13.70 0 -10 16 25.70 12.80 0 -10 16 45.10 10.90 0 10 -16 33.40 16.00 0 10 16 34.50 15.40 3 0 -17 72.79 15.20 -3 0 17 62.19 14.40 2 0 -17 0.90 10.40 2 0 -17 7.20 10.20 -2 0 17 -6.60 10.40 1 0 -17 1244.48 33.10 -1 0 17 1295.17 34.20 1 0 -17 1269.27 36.80 0 0 -17 0.30 7.00 0 0 -17 -9.40 10.90 0 0 17 1.90 9.50 0 0 17 10.60 8.60 1 0 17 79.49 9.10 1 0 17 69.99 11.60 -1 0 -17 92.49 13.80 -2 0 -17 -0.50 5.30 2 0 17 1.00 7.10 2 0 17 1.50 12.20 -3 -1 17 -9.70 12.70 2 -1 -17 31.10 11.40 -2 -1 17 22.10 11.00 2 -1 -17 43.30 10.90 2 1 -17 19.10 13.00 2 1 -17 44.20 10.90 -2 1 17 34.50 9.60 -1 -1 17 83.19 11.10 1 -1 -17 100.79 11.00 1 -1 -17 108.79 13.10 -1 1 17 87.29 12.50 1 1 -17 78.29 10.10 1 1 -17 88.89 12.70 0 -1 -17 7.60 10.30 0 -1 17 17.60 8.60 0 -1 17 -21.20 8.90 0 -1 -17 -7.30 7.20 0 1 -17 -2.30 10.40 0 1 -17 -2.90 7.50 0 1 17 3.10 9.80 0 1 17 23.90 9.80 1 -1 17 153.38 12.70 1 -1 17 139.19 13.40 -1 -1 -17 131.59 13.60 1 1 17 124.79 13.40 1 1 17 137.89 11.90 -1 1 -17 144.69 11.20 -1 1 -17 110.79 14.40 -2 -1 -17 208.78 10.40 2 -1 17 216.78 19.20 2 -1 17 210.68 13.00 2 1 17 217.68 19.80 -2 1 -17 198.38 11.60 2 -2 -17 49.90 12.20 2 -2 -17 52.99 11.20 -2 -2 17 56.59 12.10 2 2 -17 42.40 12.20 2 2 -17 67.59 11.70 -1 -2 17 134.29 13.20 1 -2 -17 181.48 18.30 1 -2 -17 152.48 12.10 1 2 -17 121.29 11.70 1 2 -17 163.88 15.20 0 -2 -17 106.89 13.20 0 -2 17 87.29 11.10 0 -2 -17 119.39 10.00 0 -2 17 79.09 11.40 0 2 -17 103.69 9.60 0 2 -17 80.19 13.60 0 2 17 98.59 13.30 -1 -2 -17 6.80 7.00 1 -2 17 -0.90 9.40 1 -2 17 16.20 8.20 -1 2 -17 8.50 6.70 1 2 17 7.50 9.70 -1 2 -17 4.80 11.10 -2 -2 -17 130.19 8.80 2 -2 17 128.19 10.00 2 -2 17 127.49 14.00 2 2 17 129.49 14.90 -2 2 -17 132.39 11.80 -2 -3 17 60.49 11.10 2 -3 -17 81.49 13.10 2 -3 -17 64.19 12.00 2 3 -17 57.59 13.00 2 3 -17 47.10 10.00 -1 -3 17 320.27 18.90 1 -3 -17 330.57 17.20 1 -3 -17 334.37 21.40 1 3 -17 273.67 16.80 1 3 -17 301.77 22.00 0 -3 17 1.30 7.90 0 -3 -17 6.60 9.70 0 -3 17 14.10 9.60 0 -3 -17 -0.40 7.10 0 3 17 4.60 10.70 0 3 -17 17.20 11.80 0 3 -17 7.00 8.50 1 -3 17 231.38 18.20 -1 -3 -17 254.17 14.90 1 -3 17 215.58 15.80 -1 3 -17 220.28 20.90 -1 3 -17 225.28 13.40 1 3 17 271.97 20.00 -2 -3 -17 15.60 4.60 2 -3 17 14.80 7.20 2 -3 17 15.80 12.00 2 3 17 15.90 12.20 -2 -4 17 -2.10 11.00 2 -4 -17 3.50 11.30 2 -4 -17 -9.50 10.00 2 4 -17 11.90 12.00 1 -4 -17 75.79 10.50 -1 -4 17 71.69 11.70 1 -4 -17 66.49 12.80 1 4 -17 64.39 10.10 1 4 -17 71.29 13.70 0 -4 -17 82.09 8.50 0 -4 17 82.09 12.40 0 -4 17 94.79 10.60 0 -4 -17 87.39 13.20 0 4 17 77.19 13.60 0 4 -17 86.49 9.60 0 4 -17 86.69 14.10 1 -4 17 7.10 9.40 -1 -4 -17 14.30 6.10 1 -4 17 16.90 9.00 -1 4 -17 14.50 6.50 1 4 17 10.90 10.80 -1 4 -17 14.10 11.60 2 -4 17 123.89 10.70 2 -4 17 124.09 14.40 -2 -4 -17 110.69 7.80 -2 4 -17 130.49 12.10 2 4 17 117.39 14.70 2 -5 -17 75.19 13.10 -2 -5 17 115.59 14.20 2 -5 -17 89.59 15.70 2 5 -17 100.69 14.60 1 -5 -17 -8.40 8.50 1 -5 -17 -7.30 11.10 -1 -5 17 0.10 9.50 1 5 -17 -6.60 7.30 1 5 -17 17.20 12.50 0 -5 -17 49.99 7.70 0 -5 -17 39.60 12.20 0 -5 17 58.79 10.30 0 -5 17 56.79 11.80 0 5 -17 67.09 13.30 0 5 -17 63.89 9.40 0 5 17 51.69 12.70 -1 -5 -17 160.38 11.10 1 -5 17 179.78 15.60 1 -5 17 153.38 14.70 -1 5 -17 140.99 16.10 1 5 17 152.58 15.30 -1 5 -17 153.78 13.00 2 -6 -17 -13.70 10.80 -2 -6 17 -0.40 11.80 2 -6 -17 -7.10 12.30 2 6 -17 -5.90 12.70 -1 -6 17 8.70 10.00 1 -6 -17 0.60 10.50 1 -6 -17 12.50 11.80 1 6 -17 14.40 12.80 1 6 -17 13.50 7.80 0 -6 17 18.30 9.50 0 -6 -17 20.60 11.90 0 -6 -17 4.20 8.10 0 -6 17 15.30 10.70 0 6 -17 7.60 9.10 0 6 -17 -20.70 12.50 0 6 17 10.50 11.70 -1 -6 -17 1.30 8.80 1 -6 17 -1.40 8.20 -1 -6 -17 3.80 6.10 1 -6 17 7.40 9.90 -1 6 -17 -24.50 12.60 1 6 17 8.20 12.10 -1 6 -17 9.50 7.70 1 -7 -17 0.50 11.90 -1 -7 17 -7.50 10.40 1 -7 -17 13.90 10.60 1 7 -17 8.10 14.00 1 7 -17 4.20 9.80 0 -7 17 33.50 11.30 0 -7 -17 18.00 12.10 0 -7 17 34.10 10.40 0 -7 -17 50.79 9.50 0 7 -17 41.50 10.20 0 7 17 13.00 13.40 0 7 -17 58.59 15.00 1 -7 17 127.19 14.90 1 -7 17 153.78 13.10 -1 -7 -17 126.89 11.20 -1 -7 -17 106.39 13.30 1 7 17 111.49 17.50 -1 7 -17 138.79 11.90 -1 -8 17 10.60 10.80 1 -8 -17 -9.50 12.60 1 -8 -17 7.30 10.00 1 8 -17 1.80 13.90 -1 8 17 -0.40 13.70 0 -8 -17 96.69 14.80 0 -8 17 53.29 13.80 0 -8 17 97.89 12.90 0 -8 -17 100.29 10.50 0 8 -17 98.69 16.20 0 8 17 86.09 15.90 0 8 -17 79.19 12.10 -2 0 18 284.47 21.70 2 0 -18 262.67 22.40 1 0 -18 -3.70 8.80 -1 0 18 -7.70 10.10 1 0 -18 -4.70 12.10 0 0 18 93.69 10.70 0 0 -18 101.49 14.50 0 0 18 115.69 13.90 0 0 -18 98.19 10.40 1 0 18 -21.60 9.90 -1 0 -18 -6.80 11.40 1 0 18 -3.60 8.30 2 -1 -18 -1.10 11.60 2 -1 -18 4.40 11.90 -2 -1 18 23.00 12.40 -2 1 18 16.10 11.60 2 1 -18 -2.90 12.20 1 -1 -18 368.56 18.70 -1 -1 18 379.26 20.70 1 -1 -18 347.77 23.80 1 1 -18 311.27 23.60 1 1 -18 353.06 19.00 -1 1 18 379.26 20.30 0 -1 -18 7.50 7.10 0 -1 -18 6.70 11.90 0 -1 18 2.30 10.90 0 -1 18 1.50 10.10 0 1 18 2.60 8.90 0 1 18 -1.70 10.90 0 1 -18 11.60 12.30 0 1 -18 9.40 7.40 1 -1 18 -10.20 8.30 -1 -1 -18 18.80 11.40 1 -1 18 -0.10 11.10 1 1 18 1.90 7.60 -1 1 -18 1.90 8.60 -1 1 -18 -19.00 11.20 1 1 18 -21.70 10.60 2 -2 -18 38.90 13.80 -2 -2 18 36.40 12.40 2 -2 -18 55.59 13.80 2 2 -18 42.50 13.10 1 -2 -18 236.38 21.40 1 -2 -18 248.18 17.00 -1 -2 18 246.78 18.30 1 2 -18 193.98 18.00 1 2 -18 235.78 16.90 0 -2 18 11.30 8.50 0 -2 -18 23.20 11.90 0 -2 18 20.20 12.00 0 -2 -18 32.10 7.80 0 2 -18 24.90 8.20 0 2 -18 22.40 12.90 0 2 18 -5.40 11.20 -1 -2 -18 150.28 12.60 1 -2 18 146.39 14.70 1 2 18 163.28 16.00 -1 2 -18 112.69 15.40 -1 2 -18 172.28 13.20 2 -3 -18 1.00 12.70 2 -3 -18 -3.80 12.90 -2 -3 18 -4.00 11.70 2 3 -18 -13.70 13.10 1 -3 -18 60.29 11.60 1 -3 -18 48.40 13.40 -1 -3 18 53.59 11.10 1 3 -18 48.00 10.70 1 3 -18 51.49 14.70 0 -3 -18 -7.70 11.60 0 -3 18 0.70 10.10 0 -3 18 1.10 10.90 0 -3 -18 -1.00 7.90 0 3 -18 4.50 8.30 0 3 18 2.00 11.70 0 3 -18 7.30 12.60 1 -3 18 -11.30 8.60 -1 -3 -18 -1.00 5.80 1 -3 18 5.60 10.80 -1 3 -18 -22.30 13.70 -1 3 -18 11.70 7.90 1 3 18 -10.50 11.90 -1 -4 18 -12.50 10.00 1 -4 -18 -12.40 8.80 1 -4 -18 -6.70 12.20 1 4 -18 16.00 13.50 1 4 -18 -9.90 9.70 0 -4 18 60.89 12.20 0 -4 -18 56.29 9.40 0 -4 -18 53.89 13.00 0 -4 18 40.10 12.30 0 4 -18 55.79 9.50 0 4 -18 55.09 14.50 0 4 18 31.90 13.20 1 -4 18 38.90 12.30 -1 -4 -18 23.10 6.60 1 -4 18 24.10 9.70 -1 4 -18 -3.00 8.30 1 4 18 38.70 13.30 1 -5 -18 243.58 23.00 -1 -5 18 221.28 20.20 1 -5 -18 209.78 17.40 1 5 -18 242.98 24.30 1 5 -18 238.58 18.10 0 -5 18 22.80 11.40 0 -5 18 22.40 9.90 0 -5 -18 14.90 13.00 0 -5 -18 35.80 8.60 0 5 18 7.10 12.20 0 5 -18 -2.70 13.80 0 5 -18 5.50 9.20 -1 -6 18 64.39 12.60 1 -6 -18 71.79 11.60 1 -6 -18 41.30 14.00 -1 6 18 78.99 16.20 1 6 -18 60.09 15.70 0 -6 18 26.00 10.50 0 -6 -18 7.20 7.40 0 -6 18 20.00 12.30 0 -6 -18 4.50 13.10 0 6 18 5.50 13.60 0 6 -18 1.50 14.20 0 6 -18 -2.40 9.40 -1 0 19 352.36 21.10 1 0 -19 258.97 18.70 1 0 -19 311.47 24.90 0 0 -19 21.60 8.00 0 0 19 10.10 11.90 0 0 -19 -1.40 12.90 0 0 19 -9.50 10.60 1 -1 -19 194.38 16.60 -1 -1 19 196.88 16.10 1 -1 -19 181.68 17.60 1 1 -19 199.88 17.60 -1 1 19 211.78 18.70 1 1 -19 172.08 17.90 0 -1 -19 154.58 13.10 0 -1 -19 162.78 17.20 0 -1 19 187.68 18.90 0 -1 19 189.68 14.90 0 1 19 146.49 12.70 0 1 19 181.28 17.10 0 1 -19 198.38 14.70 0 1 -19 165.68 17.30 0 -2 -19 199.98 18.80 0 -2 19 234.18 17.70 0 -2 -19 237.58 15.90 0 -2 19 260.17 23.00 0 2 19 263.07 23.40 0 2 -19 240.38 24.40 0 2 -19 235.88 16.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 16337 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.08492(8) 0.40501(3) 0.92348(3) 0.02094(14) Uani 1 1 d . . . . . O1 O -0.0261(2) 0.44708(7) 0.40305(7) 0.0157(2) Uani 1 1 d . . . . . H1 H 0.033621 0.409767 0.368203 0.024 Uiso 1 1 calc R U . . . N51 N 0.0712(3) 0.35393(8) 0.57680(8) 0.0140(3) Uani 1 1 d . . . . . H51 H 0.119655 0.409570 0.581530 0.017 Uiso 1 1 calc R U . . . N1 N 0.4719(3) 0.16728(9) 0.75696(9) 0.0176(3) Uani 1 1 d . . . . . C8 C 0.8315(3) 0.37200(11) 0.83833(10) 0.0147(3) Uani 1 1 d . . . . . C9 C 0.7533(3) 0.28380(10) 0.83011(10) 0.0150(3) Uani 1 1 d . . . . . H9 H 0.838362 0.241350 0.869170 0.018 Uiso 1 1 calc R U . . . C10 C 0.5425(3) 0.25698(10) 0.76205(10) 0.0137(3) Uani 1 1 d . . . . . C5 C 0.4152(3) 0.32266(10) 0.70319(10) 0.0126(3) Uani 1 1 d . . . . . C4 C 0.2010(3) 0.29372(10) 0.63409(10) 0.0130(3) Uani 1 1 d . . . . . C52 C -0.1484(3) 0.32716(10) 0.50728(10) 0.0143(3) Uani 1 1 d . . . . . H52A H -0.313623 0.300096 0.534654 0.017 Uiso 1 1 calc R U . . . H52B H -0.066247 0.282915 0.468383 0.017 Uiso 1 1 calc R U . . . C53 C -0.2502(3) 0.40823(10) 0.45255(10) 0.0153(3) Uani 1 1 d . . . . . H53A H -0.411136 0.390514 0.411165 0.018 Uiso 1 1 calc R U . . . H53B H -0.322756 0.453223 0.492527 0.018 Uiso 1 1 calc R U . . . C2 C 0.2813(3) 0.14390(10) 0.69095(11) 0.0180(3) Uani 1 1 d . . . . . H2 H 0.235029 0.083268 0.685737 0.022 Uiso 1 1 calc R U . . . C3 C 0.1435(3) 0.20199(10) 0.62848(10) 0.0159(3) Uani 1 1 d . . . . . H3 H 0.014301 0.179667 0.583476 0.019 Uiso 1 1 calc R U . . . C6 C 0.5070(3) 0.41296(10) 0.71341(10) 0.0154(3) Uani 1 1 d . . . . . H6 H 0.426774 0.456279 0.674428 0.018 Uiso 1 1 calc R U . . . C7 C 0.7116(3) 0.43807(10) 0.77953(10) 0.0154(3) Uani 1 1 d . . . . . H7 H 0.770152 0.497660 0.785419 0.018 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0218(2) 0.0217(2) 0.0185(2) 0.00085(15) -0.00591(15) -0.00028(15) O1 0.0209(5) 0.0105(5) 0.0157(5) -0.0011(4) -0.0002(4) -0.0010(4) N51 0.0170(6) 0.0098(6) 0.0150(6) 0.0005(5) -0.0013(5) -0.0007(5) N1 0.0206(6) 0.0131(7) 0.0193(7) 0.0043(5) 0.0023(5) 0.0003(5) C8 0.0136(7) 0.0177(8) 0.0129(7) 0.0000(6) 0.0008(5) 0.0012(6) C9 0.0149(7) 0.0158(8) 0.0147(7) 0.0051(6) 0.0036(6) 0.0036(6) C10 0.0146(7) 0.0136(8) 0.0135(7) 0.0035(6) 0.0061(6) 0.0020(6) C5 0.0126(7) 0.0129(7) 0.0127(7) 0.0007(6) 0.0040(5) 0.0019(5) C4 0.0136(7) 0.0133(7) 0.0124(7) 0.0007(6) 0.0044(5) 0.0023(5) C52 0.0144(7) 0.0140(7) 0.0144(7) -0.0014(6) 0.0010(5) -0.0015(6) C53 0.0151(7) 0.0133(7) 0.0172(7) -0.0025(6) -0.0020(6) 0.0015(5) C2 0.0221(8) 0.0108(7) 0.0214(8) 0.0014(6) 0.0039(6) -0.0012(6) C3 0.0182(7) 0.0150(8) 0.0147(7) -0.0008(6) 0.0023(6) -0.0012(6) C6 0.0183(7) 0.0129(8) 0.0151(7) 0.0028(6) 0.0009(6) 0.0026(6) C7 0.0167(7) 0.0117(7) 0.0179(8) 0.0002(6) 0.0010(6) -0.0001(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C53 O1 H1 109.5 . . ? C4 N51 C52 121.86(13) . . ? C4 N51 H51 119.1 . . ? C52 N51 H51 119.1 . . ? C2 N1 C10 116.04(13) . . ? C9 C8 C7 121.74(14) . . ? C9 C8 Cl1 119.83(12) . . ? C7 C8 Cl1 118.43(12) . . ? C8 C9 C10 119.98(14) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? N1 C10 C9 117.47(13) . . ? N1 C10 C5 123.35(13) . . ? C9 C10 C5 119.18(14) . . ? C6 C5 C10 118.75(13) . . ? C6 C5 C4 123.01(13) . . ? C10 C5 C4 118.23(13) . . ? N51 C4 C3 122.54(14) . . ? N51 C4 C5 120.49(13) . . ? C3 C4 C5 116.94(14) . . ? N51 C52 C53 110.06(12) . . ? N51 C52 H52A 109.6 . . ? C53 C52 H52A 109.6 . . ? N51 C52 H52B 109.6 . . ? C53 C52 H52B 109.6 . . ? H52A C52 H52B 108.2 . . ? O1 C53 C52 113.32(12) . . ? O1 C53 H53A 108.9 . . ? C52 C53 H53A 108.9 . . ? O1 C53 H53B 108.9 . . ? C52 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? N1 C2 C3 125.91(14) . . ? N1 C2 H2 117.0 . . ? C3 C2 H2 117.0 . . ? C4 C3 C2 119.45(14) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C7 C6 C5 121.50(14) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 118.82(14) . . ? C6 C7 H7 120.6 . . ? C8 C7 H7 120.6 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C8 1.7408(15) . ? O1 C53 1.4245(19) . ? O1 H1 0.8200 . ? N51 C4 1.3526(19) . ? N51 C52 1.4577(18) . ? N51 H51 0.8600 . ? N1 C2 1.324(2) . ? N1 C10 1.376(2) . ? C8 C9 1.366(2) . ? C8 C7 1.409(2) . ? C9 C10 1.417(2) . ? C9 H9 0.9300 . ? C10 C5 1.417(2) . ? C5 C6 1.415(2) . ? C5 C4 1.447(2) . ? C4 C3 1.393(2) . ? C52 C53 1.516(2) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C2 C3 1.396(2) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C6 C7 1.372(2) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C8 C9 C10 -1.1(2) . . . . ? Cl1 C8 C9 C10 178.66(11) . . . . ? C2 N1 C10 C9 -177.94(13) . . . . ? C2 N1 C10 C5 2.1(2) . . . . ? C8 C9 C10 N1 -179.94(14) . . . . ? C8 C9 C10 C5 0.0(2) . . . . ? N1 C10 C5 C6 -179.00(14) . . . . ? C9 C10 C5 C6 1.1(2) . . . . ? N1 C10 C5 C4 -0.2(2) . . . . ? C9 C10 C5 C4 179.86(13) . . . . ? C52 N51 C4 C3 2.7(2) . . . . ? C52 N51 C4 C5 -179.11(12) . . . . ? C6 C5 C4 N51 -1.9(2) . . . . ? C10 C5 C4 N51 179.37(13) . . . . ? C6 C5 C4 C3 176.37(14) . . . . ? C10 C5 C4 C3 -2.4(2) . . . . ? C4 N51 C52 C53 -178.94(13) . . . . ? N51 C52 C53 O1 64.93(16) . . . . ? C10 N1 C2 C3 -1.5(2) . . . . ? N51 C4 C3 C2 -178.79(14) . . . . ? C5 C4 C3 C2 3.0(2) . . . . ? N1 C2 C3 C4 -1.1(2) . . . . ? C10 C5 C6 C7 -1.0(2) . . . . ? C4 C5 C6 C7 -179.75(14) . . . . ? C5 C6 C7 C8 -0.1(2) . . . . ? C9 C8 C7 C6 1.2(2) . . . . ? Cl1 C8 C7 C6 -178.60(12) . . . . ?