#------------------------------------------------------------------------------ #$Date: 2024-10-22 01:10:36 +0300 (Tue, 22 Oct 2024) $ #$Revision: 295572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/29/1572911.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_1572911 loop_ _publ_author_name 'Limberg, Niklas' 'Rautiainen, J. Mikko' 'Lundell, Jan' 'Riedel, Sebastian' 'Puttreddy, Rakesh R.' 'Rissanen, Kari' _publ_section_title ; Dichlorine-Pyridine N-oxide Halogen-Bonded Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC06270A _journal_year 2024 _chemical_formula_moiety 'Cl, C9 H14 N O' _chemical_formula_sum 'C9 H14 Cl N O' _chemical_formula_weight 187.66 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-09-11 _audit_creation_method ; Olex2 1.5-alpha (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-09-13 deposited with the CCDC. 2024-10-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.8661(5) _cell_length_b 10.3264(4) _cell_length_c 10.6277(6) _cell_measurement_reflns_used 9896 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 25.314 _cell_measurement_theta_min 2.751 _cell_volume 973.02(9) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _diffrn_ambient_temperature 100.00 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_unetI/netI 0.0185 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 12603 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.333 _diffrn_reflns_theta_min 2.750 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.6903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1025 before and 0.0562 after correction. The Ratio of minimum to maximum transmission is 0.9263. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.281 _exptl_crystal_description block _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.543 _exptl_crystal_size_mid 0.267 _exptl_crystal_size_min 0.253 _refine_diff_density_max 0.214 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.033 _refine_ls_abs_structure_details ; Flack x determined using 716 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 1776 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0204 _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^)+(0.0226P)^2^+0.2813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0528 _reflns_Friedel_coverage 0.701 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 1740 _reflns_number_total 1776 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06270a3.cif _cod_data_source_block OGH_D49_41 _cod_database_code 1572911 _shelx_shelxl_version_number 2019/1 _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_max 0.918 _shelx_estimated_absorpt_t_min 0.834 _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C1(H1A), C2(H2), C4(H4), C5(H5) 1.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C) 1.c Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; TITL full1_P212121_a.res in P2(1)2(1)2(1) full1_p212121_a.res created by SHELXL-2019/1 at 11:26:07 on 13-Jun-2024 REM Old TITL full1_P212121 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.073, Rweak 0.029, Alpha 0.003 REM 0.832 for 17 systematic absences, Orientation as input REM Flack x = 0.049 ( 0.020 ) from 717 Parsons' quotients REM Formula found by SHELXT: C9 Cl N O CELL 0.71073 8.8661 10.3264 10.6277 90 90 90 ZERR 4 0.0005 0.0004 0.0006 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N O UNIT 36 56 4 4 4 L.S. 10 PLAN 2 SIZE 0.253 0.267 0.543 TEMP -173.15 CONF LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.022600 0.281300 FVAR 1.41451 CL1 3 -0.058634 0.680261 0.736698 11.00000 0.01840 0.01811 = 0.02124 0.00037 0.00249 0.00205 O1 5 0.108722 0.617563 0.515665 11.00000 0.01705 0.03223 = 0.01821 0.00229 -0.00253 0.01141 AFIX 147 H1 2 0.056410 0.637037 0.578788 11.00000 -1.50000 AFIX 0 N1 4 0.236451 0.553227 0.554076 11.00000 0.01529 0.01858 = 0.01311 -0.00137 -0.00238 0.00411 C1 1 0.365648 0.585507 0.497629 11.00000 0.02149 0.01778 = 0.01536 0.00205 0.00124 -0.00051 AFIX 43 H1A 2 0.368071 0.653917 0.437896 11.00000 -1.20000 AFIX 0 C2 1 0.495002 0.518767 0.526833 11.00000 0.01567 0.01698 = 0.01634 0.00136 0.00255 -0.00056 AFIX 43 H2 2 0.586614 0.540613 0.485617 11.00000 -1.20000 AFIX 0 C4 1 0.355234 0.391213 0.672125 11.00000 0.01671 0.01483 = 0.01317 0.00054 0.00084 -0.00083 AFIX 43 H4 2 0.349604 0.324918 0.733924 11.00000 -1.20000 AFIX 0 C6 1 0.635841 0.344656 0.652578 11.00000 0.01411 0.01589 = 0.01336 -0.00095 0.00072 0.00106 C5 1 0.226916 0.457360 0.639727 11.00000 0.01468 0.01676 = 0.01498 -0.00154 0.00222 -0.00261 AFIX 43 H5 2 0.132802 0.435957 0.677055 11.00000 -1.20000 AFIX 0 C3 1 0.494392 0.419227 0.616126 11.00000 0.01638 0.01299 = 0.01109 -0.00415 -0.00066 -0.00130 C8 1 0.603506 0.198216 0.646500 11.00000 0.01973 0.01647 = 0.02512 -0.00076 -0.00257 0.00144 AFIX 137 H8A 2 0.527131 0.175654 0.709451 11.00000 -1.50000 H8B 2 0.696511 0.150094 0.663724 11.00000 -1.50000 H8C 2 0.566305 0.175739 0.562459 11.00000 -1.50000 AFIX 0 C9 1 0.678667 0.382103 0.788219 11.00000 0.01705 0.02469 = 0.01376 -0.00222 -0.00085 0.00252 AFIX 137 H9A 2 0.701445 0.474892 0.791867 11.00000 -1.50000 H9B 2 0.767561 0.332571 0.814434 11.00000 -1.50000 H9C 2 0.594248 0.362674 0.844671 11.00000 -1.50000 AFIX 0 C7 1 0.769054 0.375008 0.564934 11.00000 0.01602 0.02515 = 0.01710 0.00131 0.00203 0.00273 AFIX 137 H7A 2 0.740768 0.355315 0.477870 11.00000 -1.50000 H7B 2 0.856159 0.322134 0.589084 11.00000 -1.50000 H7C 2 0.795202 0.466934 0.571946 11.00000 -1.50000 AFIX 0 HKLF 4 REM full1_P212121_a.res in P2(1)2(1)2(1) REM wR2 = 0.0528, GooF = S = 1.088, Restrained GooF = 1.088 for all data REM R1 = 0.0204 for 1740 Fo > 4sig(Fo) and 0.0213 for all 1776 data REM 113 parameters refined using 0 restraints END WGHT 0.0226 0.2813 REM Highest difference peak 0.214, deepest hole -0.161, 1-sigma level 0.033 Q1 1 0.6106 0.2777 0.6538 11.00000 0.05 0.21 Q2 1 0.6542 0.3569 0.7146 11.00000 0.05 0.18 ; _shelx_res_checksum 52055 _shelx_hkl_file ; 1 0 0 0.60 0.40 1 0 0 0.20 0.40 -1 0 0 0.60 0.40 -1 0 0 0.10 0.50 -2 0 0 51.29 4.30 -2 0 0 54.39 4.10 2 0 0 55.79 4.40 2 0 0 63.39 4.20 -3 0 0 -0.80 1.20 -3 0 0 0.90 1.40 3 0 0 1.30 1.40 3 0 0 3.20 1.70 4 0 0 22.90 4.10 4 0 0 22.90 4.60 -4 0 0 20.80 4.20 -4 0 0 31.20 5.30 5 0 0 -0.20 2.10 5 0 0 1.00 1.60 -5 0 0 -1.80 2.10 -5 0 0 -2.70 2.00 -6 0 0 727.43 32.30 -6 0 0 681.03 29.60 6 0 0 675.23 29.00 6 0 0 680.63 26.80 -6 0 0 711.73 28.60 -7 0 0 4.80 4.70 -7 0 0 -0.70 3.40 7 0 0 0.30 2.60 -7 0 0 -2.10 3.70 7 0 0 6.70 4.40 -8 0 0 370.96 23.20 -8 0 0 378.96 25.20 8 0 0 442.46 26.10 8 0 0 409.86 22.20 -9 0 0 -10.40 5.50 -9 0 0 4.70 6.30 9 0 0 2.00 4.60 10 0 0 316.17 21.50 -10 0 0 294.47 24.90 -10 0 0 277.97 27.70 -10 0 0 258.77 23.90 0 -1 0 0.60 0.20 0 1 0 -0.10 0.20 -1 1 0 2405.16 61.49 -1 -1 0 2537.05 66.49 1 1 0 2422.56 65.79 1 -1 0 2432.06 61.69 2 1 0 6470.65 160.48 -2 -1 0 6079.49 158.78 -3 -1 0 2.60 2.10 -3 1 0 3.10 1.70 3 -1 0 6.70 1.90 3 1 0 3.80 1.90 3 1 0 4.50 2.00 3 -1 0 4.30 1.80 -3 -1 0 3.40 1.90 4 1 0 2485.65 64.49 4 -1 0 2419.56 64.29 -4 1 0 2487.55 63.59 4 1 0 2452.15 66.19 -4 1 0 2362.36 64.79 4 -1 0 2433.06 62.09 -4 -1 0 2449.16 66.19 -4 -1 0 2537.55 65.19 -4 -1 0 2392.66 67.49 -5 -1 0 160.88 12.00 5 1 0 178.58 12.80 -5 -1 0 163.78 13.30 -5 -1 0 162.78 11.70 -5 1 0 190.08 12.70 -5 1 0 186.38 11.80 5 -1 0 184.38 10.70 5 -1 0 169.48 11.80 5 1 0 181.68 11.80 6 -1 0 537.65 22.30 6 1 0 573.44 24.30 -6 -1 0 534.85 24.60 -6 -1 0 525.25 27.20 -6 1 0 548.65 27.30 -6 -1 0 522.55 25.40 6 1 0 546.45 26.00 -6 1 0 552.44 24.20 -6 1 0 575.04 25.90 -7 1 0 1043.20 39.40 -7 -1 0 1042.30 44.30 -7 -1 0 1075.29 40.60 -7 1 0 1108.99 44.70 7 1 0 1022.40 41.30 -7 1 0 1013.10 40.70 -7 -1 0 1006.00 41.10 7 -1 0 1044.60 36.50 7 -1 0 1051.19 40.10 7 1 0 1066.89 38.70 -8 -1 0 106.19 13.10 -8 -1 0 149.49 16.00 8 -1 0 116.59 11.10 -8 1 0 141.59 15.10 -8 1 0 130.29 13.50 8 1 0 127.89 13.00 8 -1 0 141.19 14.30 -8 1 0 130.59 16.00 -9 1 0 404.36 29.10 9 1 0 343.97 21.90 -9 -1 0 348.07 25.80 -9 1 0 375.06 25.30 -9 -1 0 327.47 23.90 9 -1 0 341.97 20.60 9 -1 0 343.17 23.90 -9 1 0 362.06 26.80 10 -1 0 289.67 23.40 -10 -1 0 289.67 23.80 -10 -1 0 290.27 25.70 10 1 0 245.38 20.50 -10 1 0 248.98 26.20 -10 -1 0 248.38 26.70 10 -1 0 260.17 19.00 -10 1 0 231.68 21.40 -10 1 0 225.88 21.80 0 2 0 718.13 18.20 0 -2 0 733.93 18.10 0 2 0 732.93 18.10 0 -2 0 740.23 17.40 2 -2 0 2564.14 59.39 -2 -2 0 2592.54 64.39 2 2 0 2618.54 64.79 -2 -2 0 2568.74 64.29 2 2 0 2574.94 63.29 2 -2 0 2522.25 61.29 -2 2 0 2610.64 60.39 2 -2 0 2629.04 58.79 -2 -2 0 2656.93 63.49 -2 2 0 2421.66 61.89 -2 2 0 2628.24 61.79 3 -2 0 4.70 1.50 -3 -2 0 2.70 1.70 -3 2 0 3.70 1.80 3 2 0 2.80 2.20 -3 2 0 4.00 1.60 -3 -2 0 5.90 2.40 -3 -2 0 2.40 2.30 3 -2 0 5.80 1.80 4 -2 0 2718.73 69.69 4 -2 0 2729.93 70.19 -4 -2 0 2737.43 74.59 -4 2 0 2708.73 71.29 -4 -2 0 2774.12 73.79 -4 2 0 2661.93 69.09 4 2 0 2754.72 73.99 4 -2 0 2778.92 67.09 4 2 0 2787.72 71.99 -4 -2 0 2706.63 71.89 -5 2 0 235.18 14.20 -5 -2 0 247.08 15.60 -5 -2 0 223.48 14.30 5 -2 0 241.38 11.90 5 -2 0 242.48 13.80 -5 2 0 227.78 13.00 5 2 0 255.17 16.00 5 2 0 249.48 14.60 5 -2 0 249.08 13.70 -5 -2 0 239.58 15.90 -6 -2 0 493.25 24.10 -6 -2 0 506.25 25.20 6 -2 0 466.35 22.10 -6 2 0 483.75 22.30 6 -2 0 489.95 19.80 -6 -2 0 461.05 25.40 6 2 0 487.75 24.90 6 -2 0 478.85 22.10 -6 2 0 455.05 23.00 6 2 0 461.45 22.30 7 -2 0 -0.50 3.70 -7 -2 0 3.30 5.50 -7 2 0 6.60 3.90 7 -2 0 -6.50 3.20 -7 -2 0 -2.30 5.20 -7 -2 0 1.20 3.90 -7 2 0 0.70 3.80 7 2 0 1.30 2.60 7 -2 0 8.50 4.00 -7 2 0 5.90 4.30 8 2 0 1314.47 48.60 -8 2 0 1395.36 55.19 8 -2 0 1308.67 43.60 8 -2 0 1288.07 48.30 8 -2 0 1289.97 47.70 -8 2 0 1327.77 51.59 -8 2 0 1350.66 49.10 -8 -2 0 1361.06 56.19 -8 -2 0 1327.67 52.29 9 -2 0 666.83 29.00 9 -2 0 697.93 33.80 -9 2 0 658.73 38.20 -9 -2 0 680.33 40.40 -9 2 0 657.13 33.70 9 2 0 664.13 33.20 9 -2 0 664.23 34.00 -9 -2 0 720.63 38.20 -9 2 0 734.53 37.60 -10 2 0 215.58 25.20 10 -2 0 190.38 20.80 -10 -2 0 226.08 23.90 -10 2 0 227.68 20.80 10 -2 0 233.08 17.10 -10 -2 0 200.88 23.30 -10 -2 0 211.38 25.10 -10 2 0 218.18 23.20 10 2 0 215.58 19.60 0 -3 0 0.40 0.40 0 3 0 2.80 0.90 0 -3 0 2.20 0.90 0 3 0 1.10 0.70 -1 -3 0 3765.62 89.39 -1 3 0 3893.21 88.39 2 3 0 779.12 24.10 -2 3 0 751.62 22.60 -2 -3 0 803.82 25.30 -2 -3 0 733.73 24.40 -2 3 0 793.22 21.50 -2 3 0 759.92 20.60 -2 -3 0 779.72 23.90 -3 3 0 115.09 7.70 3 -3 0 124.89 7.30 -3 -3 0 133.29 9.60 -3 3 0 125.59 7.80 -3 -3 0 131.49 9.50 -3 3 0 114.89 6.60 -3 -3 0 115.49 8.20 3 -3 0 117.59 4.50 3 -3 0 115.59 4.80 -4 -3 0 1241.58 40.30 -4 -3 0 1229.18 40.80 4 -3 0 1224.18 31.80 4 -3 0 1195.28 35.70 -4 3 0 1211.68 35.20 4 -3 0 1200.78 39.00 -4 -3 0 1152.58 38.10 -4 3 0 1275.97 37.80 4 3 0 1219.48 38.50 -5 -3 0 3658.23 101.49 5 -3 0 3813.92 90.09 -5 3 0 3746.93 94.69 5 3 0 3827.42 98.29 -5 3 0 3585.24 96.59 -5 -3 0 3910.11 101.19 -5 -3 0 3718.03 98.29 5 -3 0 3893.51 92.89 5 -3 0 3699.63 94.79 -6 3 0 19.00 5.20 -6 -3 0 8.20 4.40 -6 3 0 15.20 5.10 -6 -3 0 11.80 5.50 6 -3 0 16.10 3.30 6 3 0 17.50 5.30 -6 -3 0 28.20 7.60 6 -3 0 8.70 3.70 6 -3 0 15.50 4.10 7 3 0 431.96 23.70 -7 -3 0 453.05 25.00 7 -3 0 422.56 18.50 7 -3 0 443.66 21.50 -7 -3 0 473.15 26.70 -7 -3 0 451.35 27.70 -7 3 0 442.56 26.00 -7 3 0 409.36 26.10 -7 3 0 479.35 25.40 7 -3 0 438.76 22.70 -8 3 0 124.99 15.40 -8 -3 0 126.39 16.30 8 3 0 114.49 13.30 8 -3 0 122.99 12.30 8 -3 0 130.79 10.40 8 -3 0 108.19 12.30 -8 3 0 139.59 15.20 -8 3 0 129.49 13.80 -8 -3 0 134.49 15.40 -9 3 0 36.50 9.70 -9 3 0 62.79 13.80 -9 -3 0 30.80 11.50 -9 -3 0 49.10 10.50 -9 3 0 50.89 9.50 9 -3 0 35.90 9.30 9 -3 0 38.40 7.80 9 -3 0 56.29 10.90 9 3 0 46.70 10.70 10 3 0 45.30 11.20 -10 3 0 35.00 10.80 -10 -3 0 27.80 15.40 -10 3 0 29.40 10.70 10 -3 0 36.00 7.70 -10 -3 0 29.40 11.30 -1 -4 0 1810.22 44.30 -1 -4 0 1690.33 46.40 1 4 0 1763.72 43.80 1 4 0 1813.12 45.60 -1 4 0 1823.82 42.40 -1 -4 0 1730.93 45.20 -2 -4 0 253.37 12.90 2 4 0 249.78 12.10 -2 -4 0 271.27 12.10 -2 4 0 271.57 11.10 -2 -4 0 257.17 12.50 -2 4 0 267.77 9.80 -3 -4 0 72.59 7.50 3 4 0 67.19 6.80 -3 -4 0 57.99 6.70 -3 4 0 70.89 6.00 -3 -4 0 64.49 6.60 3 -4 0 64.09 5.60 -3 4 0 66.39 5.10 -3 4 0 64.69 5.50 -4 -4 0 2232.98 64.09 4 -4 0 2422.56 60.49 4 4 0 2287.77 64.59 -4 -4 0 2343.17 67.29 -4 4 0 2311.37 60.19 -4 4 0 2324.07 62.89 -4 -4 0 2400.46 66.99 -5 4 0 160.08 10.80 -5 -4 0 182.18 14.30 5 -4 0 168.98 6.80 5 -4 0 156.58 10.50 5 -4 0 177.38 7.30 5 4 0 167.78 12.80 -5 -4 0 205.58 13.90 -5 -4 0 168.18 14.00 -6 4 0 1.10 2.90 6 -4 0 3.90 2.70 -6 -4 0 1.00 4.00 6 4 0 -2.00 3.10 -6 -4 0 3.60 3.90 6 -4 0 1.10 1.70 6 -4 0 1.00 1.60 -6 4 0 4.90 3.20 -6 -4 0 2.00 2.90 7 4 0 453.95 25.00 -7 4 0 466.35 24.90 -7 -4 0 513.55 28.40 -7 4 0 465.35 26.90 -7 -4 0 441.36 25.50 7 -4 0 484.85 19.10 7 -4 0 487.65 17.60 7 -4 0 439.76 22.10 -7 -4 0 459.15 28.80 -8 4 0 16.00 7.00 -8 -4 0 15.10 8.00 8 -4 0 11.60 4.80 -8 4 0 7.30 5.80 -8 -4 0 20.20 8.40 -8 4 0 1.90 6.00 8 4 0 16.10 6.00 8 -4 0 11.30 4.90 -9 -4 0 1001.60 47.40 9 4 0 908.61 41.80 9 -4 0 943.91 40.30 -9 4 0 1011.30 45.30 -9 4 0 918.61 46.60 9 -4 0 925.21 31.00 -9 -4 0 854.41 42.90 -10 4 0 94.69 22.30 -10 4 0 119.79 18.30 -10 -4 0 124.59 20.20 10 -4 0 111.29 12.70 10 4 0 94.09 15.60 10 -4 0 125.99 10.50 0 -5 0 2.50 1.70 0 5 0 -0.30 1.10 0 5 0 0.10 0.90 -1 -5 0 526.85 19.30 -1 5 0 511.15 16.80 -1 5 0 536.65 16.10 -1 -5 0 507.65 16.50 -1 -5 0 550.24 18.00 1 5 0 525.05 16.30 1 5 0 512.75 18.20 -2 5 0 401.86 13.60 -2 5 0 400.96 14.90 -2 -5 0 412.36 17.30 -2 -5 0 392.76 17.50 -2 -5 0 399.06 15.80 2 -5 0 403.76 14.10 -3 5 0 3477.15 86.59 3 5 0 3691.33 91.59 -3 -5 0 3660.83 92.99 -3 5 0 3473.15 87.79 -3 -5 0 3565.14 92.59 -3 -5 0 3600.94 90.19 -4 -5 0 542.85 25.20 -4 -5 0 587.84 26.40 -4 5 0 566.84 22.60 -4 -5 0 599.54 24.50 4 -5 0 572.34 20.50 -4 5 0 592.94 22.40 4 5 0 633.84 25.50 5 5 0 118.19 10.90 -5 -5 0 84.39 10.00 -5 -5 0 100.09 11.10 -5 -5 0 100.39 11.30 5 -5 0 94.29 8.10 -5 5 0 94.29 9.20 -6 -5 0 335.67 22.10 -6 5 0 340.97 19.40 6 5 0 356.66 21.10 6 -5 0 366.26 17.50 -6 -5 0 311.47 20.00 -7 5 0 60.29 10.80 7 -5 0 75.99 8.70 -7 -5 0 52.89 10.30 -7 5 0 60.29 10.20 -7 -5 0 85.59 13.30 7 5 0 67.09 11.50 -7 -5 0 61.99 12.00 -8 5 0 160.08 15.80 -8 -5 0 99.69 16.40 -8 -5 0 155.18 17.10 8 5 0 134.09 15.20 -8 5 0 137.69 16.00 8 -5 0 145.29 13.50 9 -5 0 132.39 14.00 9 5 0 118.69 16.80 -9 -5 0 138.29 18.90 -9 -5 0 113.09 23.20 -9 5 0 137.49 16.40 -9 -5 0 94.59 15.40 0 6 0 1048.00 30.10 0 6 0 1055.39 26.80 0 -6 0 1024.20 32.00 1 6 0 748.33 25.00 -1 -6 0 795.02 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-10 178.98 22.10 -4 6 10 184.38 28.50 -4 6 10 179.08 14.70 4 -6 10 197.78 24.20 4 6 10 203.08 19.50 4 6 10 128.99 23.50 -4 6 -10 124.29 20.00 -4 6 -10 159.48 23.10 -4 -6 10 164.48 25.20 4 6 10 180.98 24.40 0 -7 10 10.00 8.20 0 7 10 11.40 4.90 0 7 10 3.90 7.50 0 7 10 4.70 7.80 0 -7 10 9.40 9.90 0 7 -10 -2.40 7.90 0 -7 10 4.10 5.80 1 -7 10 192.08 17.80 -1 7 10 146.69 24.40 1 -7 10 188.18 26.30 -1 -7 -10 209.18 17.40 1 7 -10 152.78 22.20 -1 7 10 183.88 17.80 -1 7 10 175.18 13.80 1 -7 10 199.08 19.80 -1 -7 -10 185.08 26.00 -1 -7 10 191.68 26.50 -1 -7 10 166.08 17.90 1 7 10 164.88 19.90 1 7 10 183.58 15.70 1 7 10 162.58 26.00 -1 7 -10 161.88 24.30 -1 -7 10 189.08 19.40 -2 -7 -10 378.56 34.70 -2 -7 -10 449.36 27.50 2 -7 10 416.46 28.10 2 -7 10 406.86 25.50 -2 7 10 395.66 36.50 -2 7 10 427.36 24.70 2 -7 10 491.25 37.40 2 7 -10 405.86 32.00 -2 -7 10 449.56 29.70 -2 -7 10 408.36 27.90 -2 7 -10 432.56 34.40 2 7 10 407.86 35.40 -2 7 -10 446.76 39.60 2 7 10 391.66 29.90 -2 -7 10 491.45 38.80 2 7 10 439.46 24.80 0 0 11 -5.90 5.30 0 0 11 -7.00 6.60 0 0 11 5.40 7.00 -1 0 -11 294.97 27.90 -1 0 11 300.77 28.20 1 0 11 274.67 23.60 -1 0 11 284.47 24.70 -1 0 11 239.48 21.60 1 0 11 270.57 27.00 1 0 11 281.87 25.20 2 0 -11 -4.40 6.00 2 0 11 0.50 6.20 2 0 11 -1.20 6.80 -2 0 -11 19.00 12.20 -2 0 -11 -11.80 9.40 -2 0 11 -5.30 6.50 -2 0 11 4.00 7.80 -2 0 11 1.50 5.70 3 0 11 578.44 37.10 -3 0 11 573.34 37.10 -3 0 11 611.84 34.00 3 0 11 588.64 37.10 3 0 11 586.04 40.10 -3 0 11 537.95 40.40 -3 0 -11 683.03 44.10 -3 0 -11 495.65 36.00 3 0 -11 603.04 31.80 -4 0 -11 582.14 39.50 -4 0 11 553.74 32.00 4 0 11 748.23 42.10 -4 0 11 585.34 37.60 4 0 -11 649.83 32.90 -4 0 -11 550.04 42.20 4 0 11 630.04 42.30 4 0 11 619.14 39.20 -4 0 11 667.43 44.80 5 0 11 905.51 51.89 -5 0 11 932.81 43.80 5 0 11 967.00 49.90 5 0 -11 988.50 42.20 -5 0 11 1037.00 51.99 -5 0 11 1035.00 59.09 0 1 11 106.19 16.30 0 -1 11 130.49 15.80 0 1 11 140.29 22.90 0 -1 -11 127.19 19.50 0 1 -11 106.29 15.80 0 -1 -11 124.59 15.70 0 -1 11 122.99 21.20 0 1 11 110.69 16.90 0 -1 11 125.59 19.60 -1 -1 -11 134.99 22.70 -1 -1 -11 168.48 20.30 1 -1 11 121.39 20.70 -1 1 11 110.19 16.90 -1 1 11 145.19 23.40 1 -1 11 136.49 22.00 1 -1 11 154.08 18.80 1 1 -11 147.19 16.70 -1 1 11 113.89 16.50 -1 -1 11 142.39 20.40 -1 -1 11 150.78 17.20 1 1 11 137.69 19.30 -1 -1 11 136.79 21.80 1 1 11 108.39 20.10 -1 1 -11 147.09 21.40 -1 1 -11 130.79 23.20 1 1 11 129.49 16.30 2 1 -11 337.47 32.80 2 -1 11 293.27 26.90 -2 1 11 357.36 26.30 -2 -1 -11 253.67 26.40 2 -1 11 319.57 29.90 -2 1 11 313.57 30.00 2 -1 11 338.67 27.50 -2 1 11 331.27 23.40 -2 -1 11 280.07 29.10 2 1 11 265.87 23.60 -2 1 -11 280.47 27.90 2 1 11 316.97 29.80 -2 -1 11 271.67 25.00 -2 -1 11 353.56 29.10 2 1 11 266.27 27.00 -2 1 -11 329.17 28.20 -3 -1 -11 297.97 30.20 3 1 -11 310.77 23.90 -3 1 11 317.67 26.60 -3 1 11 371.56 24.90 -3 1 11 360.66 33.00 3 -1 11 311.37 27.90 3 -1 11 370.26 31.70 3 -1 11 292.17 26.40 -3 -1 -11 320.87 27.70 3 1 11 353.86 27.60 -3 1 -11 328.97 29.40 3 1 11 350.36 31.60 -3 -1 11 355.46 25.30 -3 -1 11 328.07 27.80 3 1 11 320.07 27.60 -3 -1 11 385.16 33.30 -4 -1 -11 61.19 17.70 4 -1 11 68.99 15.20 4 -1 11 47.40 11.20 -4 1 11 48.40 12.60 -4 -1 -11 65.39 16.00 -4 1 11 47.50 16.50 4 -1 11 47.10 14.00 4 1 -11 55.19 11.80 4 1 11 70.29 15.70 -4 1 -11 54.39 17.50 4 1 11 35.70 14.00 -4 -1 11 65.59 11.90 -4 -1 11 83.49 15.70 -4 1 -11 43.00 14.60 4 1 11 69.09 14.40 -4 -1 11 85.49 18.70 -5 1 11 42.40 15.40 5 -1 11 28.90 12.10 5 1 -11 27.70 9.80 -5 1 11 54.69 12.00 -5 1 11 40.30 11.30 5 -1 11 31.10 12.80 5 1 11 58.99 13.70 -5 -1 11 46.80 12.80 -5 1 -11 23.90 16.10 5 -1 -11 37.00 9.20 -5 -1 11 61.99 16.20 5 1 11 44.80 12.80 0 -2 11 1.90 8.50 0 2 11 14.90 7.40 0 2 11 5.90 7.90 0 -2 11 0.40 8.10 0 -2 -11 14.90 7.30 0 2 -11 17.60 7.00 0 2 11 12.00 7.30 1 2 -11 75.69 13.70 1 -2 11 95.79 18.30 1 -2 11 71.19 16.30 -1 -2 -11 52.29 17.30 -1 2 11 78.99 13.80 -1 2 11 81.69 17.00 1 -2 11 73.69 16.70 -1 2 11 89.49 14.00 1 2 11 73.69 13.30 1 2 11 117.89 21.40 -1 2 -11 98.59 17.00 -1 2 -11 78.99 13.80 1 2 11 66.59 13.70 -1 -2 11 69.69 14.80 -1 -2 11 95.59 16.70 -2 2 11 312.67 23.10 2 -2 11 310.87 27.20 2 -2 11 347.17 29.30 -2 -2 -11 260.57 29.40 -2 2 11 283.27 30.60 2 2 -11 303.97 25.10 2 -2 11 325.77 26.30 -2 2 11 299.07 24.50 -2 -2 -11 359.66 28.40 2 2 11 265.37 24.40 -2 -2 11 313.97 24.10 -2 -2 11 269.77 26.70 -2 2 -11 285.97 27.60 -2 2 -11 296.37 27.90 2 2 11 330.47 26.30 -2 -2 11 299.97 27.40 2 2 11 348.77 31.60 3 -2 11 358.66 28.70 3 -2 11 328.17 28.80 -3 2 11 400.36 26.60 -3 -2 -11 409.36 30.80 3 -2 11 353.16 29.80 3 2 -11 397.46 28.30 -3 -2 -11 410.56 36.30 -3 2 11 355.36 33.70 -3 2 11 411.96 28.60 3 2 11 402.76 33.60 3 2 11 429.76 30.40 -3 2 -11 391.06 32.40 -3 2 -11 429.96 34.20 -3 -2 11 420.36 34.00 -3 -2 11 444.76 33.00 3 2 11 329.97 28.30 -3 -2 11 394.96 27.30 4 -2 11 193.48 23.10 -4 2 11 186.58 24.70 -4 2 11 171.88 18.40 -4 -2 -11 145.79 28.60 4 2 -11 207.88 20.50 -4 2 11 163.28 18.10 4 -2 11 167.18 23.80 4 -2 11 147.19 21.00 -4 -2 -11 180.08 28.10 -4 -2 11 175.08 20.60 -4 -2 11 191.08 27.30 4 2 11 188.58 24.60 -4 2 -11 198.38 26.80 4 2 11 194.88 20.70 -4 -2 11 192.58 22.30 4 2 11 180.38 24.20 -4 2 -11 206.38 25.90 5 2 -11 211.88 21.90 5 -2 11 167.78 21.60 5 -2 11 203.98 23.90 -5 2 11 188.28 18.60 -5 2 11 175.98 27.40 -5 2 11 209.68 21.20 5 2 11 216.28 26.20 5 2 11 217.38 22.60 -5 -2 11 173.08 23.70 -5 2 -11 221.88 28.30 -5 -2 11 196.28 26.00 0 -3 -11 29.00 9.60 0 3 11 48.60 11.30 0 -3 -11 18.20 11.10 0 -3 11 28.00 11.30 0 3 11 17.60 8.90 0 3 -11 32.00 10.50 0 -3 11 33.60 11.30 0 3 11 3.50 8.60 -1 -3 -11 375.76 33.30 -1 3 11 401.56 27.40 1 -3 11 433.66 33.80 1 3 -11 390.56 28.60 -1 3 11 386.06 34.00 -1 3 11 361.46 26.80 1 -3 11 417.66 35.70 1 -3 11 418.36 29.20 -1 -3 11 356.86 30.60 -1 3 -11 376.36 28.90 -1 -3 11 397.16 27.90 1 3 11 428.96 28.30 1 3 11 387.66 33.80 -1 3 -11 447.96 32.20 -1 -3 11 372.26 31.40 1 3 11 381.26 27.40 -1 3 -11 382.66 30.70 -2 3 11 316.87 31.30 2 3 -11 325.87 25.80 2 -3 11 321.27 26.10 -2 -3 -11 344.67 31.50 -2 3 11 302.37 24.20 2 -3 11 344.47 28.40 -2 -3 -11 277.77 25.00 2 -3 11 329.17 29.10 -2 3 11 291.97 22.30 -2 3 -11 318.97 28.10 -2 -3 11 267.87 23.50 2 3 11 291.57 28.30 -2 3 -11 310.77 27.00 -2 3 -11 239.28 25.20 -2 -3 11 264.37 27.40 2 3 11 286.47 23.50 -2 -3 11 308.37 28.60 2 3 11 276.17 24.80 3 3 -11 144.19 20.70 -3 3 11 173.18 17.20 -3 -3 -11 143.89 18.20 3 -3 11 218.68 23.50 3 -3 11 166.58 24.30 3 -3 11 171.18 21.60 -3 3 11 156.28 17.90 -3 3 11 160.18 25.30 -3 -3 -11 171.98 25.80 -3 -3 11 145.99 22.20 3 3 11 171.28 21.50 3 3 11 195.28 20.40 -3 3 -11 181.78 22.60 -3 3 -11 176.78 21.60 3 3 11 135.39 23.40 -3 -3 11 138.79 17.40 -3 -3 11 143.89 22.80 -4 3 11 94.39 14.90 -4 3 11 129.29 15.90 4 -3 11 113.29 20.30 -4 3 11 125.29 22.30 4 -3 11 105.99 18.30 4 3 -11 106.59 18.60 4 3 11 94.09 18.20 -4 3 -11 104.69 20.90 4 3 11 128.59 21.60 -4 3 -11 140.79 22.90 -4 -3 11 121.59 20.80 -4 -3 11 127.89 19.70 0 4 -11 63.09 14.10 0 -4 11 73.79 14.40 0 -4 11 59.39 13.10 0 4 11 50.09 11.50 0 4 11 61.39 12.00 0 -4 -11 95.89 15.30 0 -4 11 68.59 16.80 0 4 11 49.30 14.70 1 -4 11 70.59 16.60 1 -4 11 49.99 12.60 1 4 -11 76.09 16.20 -1 -4 -11 75.19 13.50 -1 4 11 64.69 13.80 -1 4 11 74.49 11.70 -1 4 11 76.69 17.40 1 -4 11 78.19 18.30 -1 -4 -11 74.39 17.00 -1 4 -11 68.09 14.90 -1 -4 11 67.09 17.70 1 4 11 48.70 11.20 -1 -4 11 52.49 12.60 -1 4 -11 54.69 14.30 1 4 11 65.59 13.40 1 4 11 65.49 16.20 -1 -4 11 76.69 14.80 2 -4 11 157.98 20.40 -2 4 11 148.29 24.80 2 4 -11 145.09 21.00 -2 4 11 171.08 18.00 2 -4 11 125.09 21.00 -2 -4 -11 142.89 18.00 2 -4 11 131.09 18.80 -2 4 11 147.69 16.10 -2 -4 -11 180.78 28.20 -2 -4 11 175.28 19.10 -2 4 -11 130.99 21.30 -2 4 -11 128.39 20.70 2 4 11 145.29 24.40 2 4 11 159.98 17.30 -2 -4 11 145.59 18.40 2 4 11 174.18 20.80 -2 -4 11 132.69 22.00 -3 4 11 243.18 21.20 3 4 -11 265.97 25.10 -3 -4 -11 252.57 25.30 3 -4 11 228.28 23.20 -3 4 11 221.28 19.20 3 -4 11 261.47 24.10 -3 4 11 241.48 29.80 3 4 11 297.67 30.10 -3 4 -11 268.37 26.60 -3 4 -11 260.47 26.20 -3 -4 11 251.77 26.50 -3 -4 11 204.48 24.20 3 4 11 265.47 22.30 -3 4 -11 212.88 27.10 3 4 11 211.08 24.90 4 4 -11 29.50 11.10 -4 4 11 5.10 9.70 -4 4 11 5.70 8.20 4 -4 11 0.10 8.50 -4 4 11 18.00 7.30 4 -4 11 27.50 9.70 -4 -4 11 19.30 11.30 4 4 11 21.90 11.00 -4 4 -11 -12.40 11.20 -4 -4 11 12.90 9.00 4 4 11 17.30 7.90 0 -5 -11 87.79 16.40 0 5 11 87.59 13.60 0 5 11 102.99 15.70 0 -5 11 58.29 14.50 0 -5 11 77.39 15.40 0 5 11 67.79 16.90 0 -5 11 92.69 19.50 0 5 -11 90.59 16.20 1 5 -11 128.59 20.80 -1 5 11 126.59 17.00 1 -5 11 156.48 19.60 -1 -5 -11 100.59 21.70 -1 5 11 123.49 14.60 -1 -5 -11 132.69 16.80 1 -5 11 141.59 23.10 1 -5 11 172.18 18.80 -1 5 11 95.09 18.40 -1 5 -11 177.18 25.50 1 5 11 173.18 26.50 -1 -5 11 111.99 16.50 -1 5 -11 129.79 21.00 -1 -5 11 134.09 20.80 1 5 11 136.09 19.00 -1 -5 11 115.09 18.60 1 5 11 152.08 16.30 2 -5 11 65.49 16.40 2 5 -11 83.99 16.40 -2 5 11 42.50 12.00 -2 5 11 55.39 14.70 -2 5 11 37.70 8.80 2 -5 11 47.40 13.50 -2 -5 -11 88.99 15.10 2 -5 11 56.39 16.70 2 5 11 62.39 12.80 -2 5 -11 48.70 12.00 2 5 11 43.40 13.30 -2 -5 11 63.09 16.00 -2 5 -11 60.99 15.00 -2 5 -11 62.59 15.30 -3 5 11 245.58 20.50 3 -5 11 253.27 23.80 3 5 -11 270.07 26.80 -3 5 11 242.28 28.30 -3 5 11 264.37 20.90 3 -5 11 261.87 28.50 3 5 11 282.17 27.80 3 5 11 281.37 22.70 -3 5 -11 261.17 27.10 -3 5 -11 213.98 24.40 -3 -5 11 273.87 27.40 -3 5 -11 214.98 26.10 -3 -5 11 266.57 29.50 3 5 11 210.68 27.20 0 6 -11 427.66 32.50 0 -6 11 377.66 34.10 0 -6 11 393.36 29.60 0 6 11 356.46 23.40 0 6 11 373.96 27.20 -1 6 11 82.99 19.70 -1 6 11 94.89 13.10 -1 6 11 83.59 14.50 1 -6 11 99.19 20.90 -1 -6 -11 81.89 12.60 1 -6 11 84.89 15.20 1 6 -11 83.99 18.30 1 6 11 75.39 11.90 1 6 11 88.19 19.90 -1 -6 11 66.99 15.40 -1 -6 11 95.29 16.80 1 6 11 75.39 15.00 -1 6 -11 55.19 15.50 0 0 12 91.39 21.00 0 0 12 124.79 18.30 0 0 12 95.19 17.10 0 0 -12 117.29 19.40 -1 0 -12 222.08 25.60 -1 0 12 220.28 20.10 1 0 12 151.48 21.00 -1 0 12 186.98 21.70 1 0 12 173.48 27.30 -1 0 -12 153.08 22.10 -1 0 12 219.98 30.90 1 0 12 185.58 25.00 2 0 12 89.69 16.60 2 0 12 78.59 18.20 2 0 12 78.69 14.70 -2 0 12 72.49 13.50 -2 0 12 87.79 17.60 -2 0 12 53.19 16.50 -2 0 -12 46.90 15.40 3 0 12 1286.17 64.29 3 0 -12 1312.17 51.89 -3 0 12 1298.47 60.79 -3 0 12 1232.88 65.69 -3 0 12 1159.08 51.99 3 0 12 1365.76 62.09 0 1 -12 50.49 11.50 0 -1 -12 50.99 12.40 0 1 12 83.09 16.00 0 -1 12 75.49 15.10 0 1 12 80.79 15.50 0 -1 12 68.59 15.60 0 -1 12 73.99 15.60 0 1 12 70.29 17.70 -1 -1 -12 251.87 29.40 1 -1 12 266.37 26.60 -1 1 12 262.77 29.10 1 -1 12 254.37 23.70 1 -1 12 233.48 26.80 -1 1 12 291.97 23.70 1 1 -12 247.88 22.80 -1 -1 -12 231.28 24.40 -1 1 12 244.58 24.20 -1 -1 12 280.77 29.00 1 1 12 258.67 28.60 1 1 12 294.87 26.70 -1 -1 12 250.87 25.10 -1 1 -12 262.07 25.30 -1 1 -12 251.97 26.80 -1 -1 12 278.47 27.80 1 1 12 278.97 24.30 2 -1 12 322.87 28.80 -2 -1 -12 278.47 33.80 -2 1 12 288.87 31.90 2 1 -12 315.47 25.00 2 -1 12 310.47 30.30 -2 1 12 336.27 26.30 -2 1 12 306.87 27.20 2 1 12 299.67 31.30 -2 1 -12 317.87 31.30 -2 -1 12 314.37 32.20 -2 -1 12 359.96 30.60 2 1 12 340.67 28.00 -2 -1 12 345.67 25.50 2 1 12 322.07 27.90 -3 1 12 59.99 16.90 -3 1 12 81.39 14.60 -3 1 12 69.09 15.10 3 1 -12 66.19 14.20 3 -1 12 66.19 16.70 3 -1 12 66.39 14.60 -3 -1 12 67.19 17.90 3 1 12 87.99 17.90 -3 -1 12 70.79 16.00 -3 1 -12 71.69 17.40 3 1 12 80.39 15.80 0 -2 -12 274.57 24.00 0 2 -12 263.27 24.10 0 -2 12 216.18 23.50 0 2 12 230.28 23.20 0 2 12 271.77 30.10 0 -2 12 273.57 28.40 0 -2 12 283.17 27.90 0 2 12 274.77 23.60 -1 -2 -12 292.97 26.70 -1 2 12 335.57 26.10 -1 2 12 276.07 31.50 1 -2 12 342.37 30.70 -1 -2 -12 358.56 47.10 1 2 -12 330.77 27.00 -1 2 12 315.57 27.10 1 -2 12 304.27 29.60 -1 -2 12 326.87 29.70 -1 2 -12 318.87 27.00 -1 -2 12 296.27 28.40 -1 2 -12 292.17 31.40 -1 -2 12 326.27 29.90 1 2 12 261.77 24.70 -1 2 -12 364.86 32.20 1 2 12 303.37 31.10 1 2 12 290.27 25.30 -2 2 12 445.86 28.70 -2 2 12 413.86 30.60 2 -2 12 407.16 33.20 2 2 -12 383.16 29.10 -2 2 12 466.95 40.20 2 -2 12 330.37 30.60 2 2 12 498.45 34.30 2 2 12 388.66 30.50 -2 2 -12 371.26 34.60 2 2 12 402.46 35.90 -2 -2 12 433.46 34.70 -2 -2 12 450.95 37.40 3 2 -12 32.20 11.20 -3 2 12 26.00 10.60 -3 2 12 54.19 12.90 -3 2 12 28.10 14.50 3 -2 12 11.10 9.90 3 -2 12 19.20 9.70 3 2 12 33.90 11.80 3 2 12 51.19 15.20 -3 -2 12 40.70 14.10 -3 2 -12 30.80 13.20 -3 -2 12 20.20 12.50 0 -3 -12 275.77 23.50 0 3 -12 248.98 24.80 0 3 12 275.97 24.00 0 3 12 283.47 24.50 0 -3 12 239.98 26.70 0 -3 12 240.68 25.40 0 3 12 304.67 31.90 1 3 -12 246.18 23.70 -1 3 12 274.17 29.70 1 -3 12 227.58 25.40 -1 3 12 318.37 28.30 1 -3 12 243.38 26.00 -1 3 12 240.28 23.20 -1 -3 -12 215.48 25.80 -1 -3 12 223.98 26.00 1 3 12 269.47 25.10 1 3 12 247.58 23.70 1 3 12 242.28 27.90 -1 3 -12 245.88 24.00 -1 -3 12 261.87 27.80 -2 3 12 296.87 32.70 -2 3 12 386.26 32.90 -2 3 12 384.36 28.50 2 -3 12 430.66 33.50 2 -3 12 352.26 32.40 2 3 -12 324.17 29.60 2 3 12 415.76 36.20 -2 -3 12 409.36 35.10 -2 -3 12 386.76 34.60 2 3 12 380.16 32.30 2 3 12 430.56 30.70 -2 3 -12 334.97 30.70 0 -4 12 153.58 20.20 0 -4 -12 86.39 15.70 0 -4 12 112.59 21.10 0 4 -12 108.49 20.80 0 4 12 110.19 16.20 0 4 12 119.69 18.30 0 4 12 128.19 24.40 -1 4 12 465.25 40.70 -1 4 12 543.65 33.30 1 -4 12 513.45 40.50 1 -4 12 550.34 37.60 1 4 -12 577.94 38.80 1 4 12 572.94 35.90 -1 -4 12 519.45 40.10 -1 -4 12 550.64 38.50 -1 4 -12 567.14 40.00 1 4 12 499.55 41.40 1 4 12 527.55 33.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 96472 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl -0.05863(5) 0.68026(4) 0.73670(4) 0.01925(13) Uani 1 1 d . . . . . O1 O 0.10872(15) 0.61756(15) 0.51566(13) 0.0225(3) Uani 1 1 d . . . . . H1 H 0.056410 0.637037 0.578788 0.034 Uiso 1 1 calc R U . . . N1 N 0.23645(18) 0.55323(15) 0.55408(14) 0.0157(3) Uani 1 1 d . . . . . C1 C 0.3656(2) 0.58551(19) 0.49763(18) 0.0182(4) Uani 1 1 d . . . . . H1A H 0.368071 0.653917 0.437896 0.022 Uiso 1 1 calc R U . . . C2 C 0.4950(2) 0.51877(19) 0.52683(17) 0.0163(4) Uani 1 1 d . . . . . H2 H 0.586614 0.540613 0.485617 0.020 Uiso 1 1 calc R U . . . C4 C 0.3552(2) 0.39121(18) 0.67213(18) 0.0149(4) Uani 1 1 d . . . . . H4 H 0.349604 0.324918 0.733924 0.018 Uiso 1 1 calc R U . . . C6 C 0.6358(2) 0.34466(17) 0.65258(17) 0.0145(4) Uani 1 1 d . . . . . C5 C 0.2269(2) 0.45736(18) 0.63973(17) 0.0155(4) Uani 1 1 d . . . . . H5 H 0.132802 0.435957 0.677055 0.019 Uiso 1 1 calc R U . . . C3 C 0.4944(2) 0.41923(17) 0.61613(17) 0.0135(4) Uani 1 1 d . . . . . C8 C 0.6035(2) 0.19822(18) 0.64650(19) 0.0204(4) Uani 1 1 d . . . . . H8A H 0.527131 0.175654 0.709451 0.031 Uiso 1 1 calc R U . . . H8B H 0.696511 0.150094 0.663724 0.031 Uiso 1 1 calc R U . . . H8C H 0.566305 0.175739 0.562459 0.031 Uiso 1 1 calc R U . . . C9 C 0.6787(2) 0.3821(2) 0.78822(17) 0.0185(4) Uani 1 1 d . . . . . H9A H 0.701445 0.474892 0.791867 0.028 Uiso 1 1 calc R U . . . H9B H 0.767561 0.332571 0.814434 0.028 Uiso 1 1 calc R U . . . H9C H 0.594248 0.362674 0.844671 0.028 Uiso 1 1 calc R U . . . C7 C 0.7691(2) 0.3750(2) 0.56493(18) 0.0194(4) Uani 1 1 d . . . . . H7A H 0.740768 0.355315 0.477870 0.029 Uiso 1 1 calc R U . . . H7B H 0.856159 0.322134 0.589084 0.029 Uiso 1 1 calc R U . . . H7C H 0.795202 0.466934 0.571946 0.029 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 0.0184(2) 0.0181(2) 0.0212(2) 0.00037(18) 0.00249(18) 0.00205(18) O1 0.0171(7) 0.0322(8) 0.0182(7) 0.0023(6) -0.0025(6) 0.0114(6) N1 0.0153(8) 0.0186(8) 0.0131(7) -0.0014(7) -0.0024(6) 0.0041(7) C1 0.0215(10) 0.0178(10) 0.0154(10) 0.0021(8) 0.0012(8) -0.0005(8) C2 0.0157(8) 0.0170(9) 0.0163(9) 0.0014(8) 0.0026(8) -0.0006(7) C4 0.0167(9) 0.0148(9) 0.0132(9) 0.0005(7) 0.0008(7) -0.0008(8) C6 0.0141(9) 0.0159(10) 0.0134(9) -0.0009(7) 0.0007(7) 0.0011(7) C5 0.0147(9) 0.0168(9) 0.0150(9) -0.0015(7) 0.0022(7) -0.0026(8) C3 0.0164(9) 0.0130(9) 0.0111(8) -0.0042(7) -0.0007(7) -0.0013(7) C8 0.0197(9) 0.0165(10) 0.0251(10) -0.0008(8) -0.0026(8) 0.0014(8) C9 0.0170(9) 0.0247(10) 0.0138(10) -0.0022(8) -0.0008(8) 0.0025(8) C7 0.0160(10) 0.0252(10) 0.0171(10) 0.0013(8) 0.0020(8) 0.0027(8) 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' Cl Cl 0.1484 0.1585 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 O1 H1 109.5 . . ? C1 N1 O1 116.91(15) . . ? C1 N1 C5 122.73(17) . . ? C5 N1 O1 120.26(15) . . ? N1 C1 H1A 120.3 . . ? N1 C1 C2 119.31(17) . . ? C2 C1 H1A 120.3 . . ? C1 C2 H2 119.4 . . ? C1 C2 C3 121.25(17) . . ? C3 C2 H2 119.4 . . ? C5 C4 H4 119.3 . . ? C5 C4 C3 121.44(17) . . ? C3 C4 H4 119.3 . . ? C3 C6 C8 109.43(15) . . ? C3 C6 C9 108.33(15) . . ? C3 C6 C7 112.08(15) . . ? C9 C6 C8 109.37(16) . . ? C7 C6 C8 108.53(15) . . ? C7 C6 C9 109.07(15) . . ? N1 C5 C4 118.92(17) . . ? N1 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C2 C3 C4 116.33(17) . . ? C2 C3 C6 122.77(16) . . ? C4 C3 C6 120.89(16) . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 O1 H1 0.8400 . ? O1 N1 1.375(2) . ? N1 C1 1.335(3) . ? N1 C5 1.348(2) . ? C1 H1A 0.9500 . ? C1 C2 1.374(3) . ? C2 H2 0.9500 . ? C2 C3 1.399(3) . ? C4 H4 0.9500 . ? C4 C5 1.371(3) . ? C4 C3 1.400(3) . ? C6 C3 1.522(2) . ? C6 C8 1.540(3) . ? C6 C9 1.540(3) . ? C6 C7 1.536(3) . ? C5 H5 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 O1 N1 C1 C2 -176.02(17) . . . . ? O1 N1 C5 C4 177.19(16) . . . . ? N1 C1 C2 C3 -1.1(3) . . . . ? C1 N1 C5 C4 1.1(3) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? C1 C2 C3 C6 -178.94(17) . . . . ? C5 N1 C1 C2 0.2(3) . . . . ? C5 C4 C3 C2 0.6(3) . . . . ? C5 C4 C3 C6 -179.74(17) . . . . ? C3 C4 C5 N1 -1.5(3) . . . . ? C8 C6 C3 C2 -130.35(18) . . . . ? C8 C6 C3 C4 50.0(2) . . . . ? C9 C6 C3 C2 110.48(19) . . . . ? C9 C6 C3 C4 -69.1(2) . . . . ? C7 C6 C3 C2 -9.9(2) . . . . ? C7 C6 C3 C4 170.49(16) . . . . ?