#------------------------------------------------------------------------------ #$Date: 2024-11-22 01:30:57 +0200 (Fri, 22 Nov 2024) $ #$Revision: 296051 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249628.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_7249628 loop_ _publ_author_name 'Nath, Jitendra' 'Baruah, Jubaraj B.' _publ_section_title ; Positional isomers of (E)-2-(anthracen-9-ylmethylene)-N-(aryl)hydrazinecarbothioamide, zinc complexes and polymorphic solvates ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00992D _journal_year 2024 _chemical_formula_moiety 'C22 H15 Cl2 N3 S' _chemical_formula_sum 'C22 H15 Cl2 N3 S' _chemical_formula_weight 424.33 _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 _audit_creation_date 2023-11-17 _audit_creation_method ; Olex2 1.5-beta (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-09-28 deposited with the CCDC. 2024-11-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.79(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.968(2) _cell_length_b 19.460(11) _cell_length_c 25.084(13) _cell_measurement_reflns_used 5508 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 20.24 _cell_measurement_theta_min 2.65 _cell_volume 1936.0(18) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _diffrn_ambient_temperature 297.00 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1226 _diffrn_reflns_av_unetI/netI 0.1330 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 18584 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.325 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5481 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1563 before and 0.0849 after correction. The Ratio of minimum to maximum transmission is 0.7355. The \l/2 correction factor is Not present. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description needle _exptl_crystal_F_000 872 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.642 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 3411 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.1621 _refine_ls_R_factor_gt 0.0778 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+1.9827P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1701 _refine_ls_wR_factor_ref 0.2131 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1805 _reflns_number_total 3411 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00992d2.cif _cod_data_source_block 23Cl_HATU _cod_original_cell_volume 1936.2(19) _cod_database_code 7249628 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2.a Aromatic/amide H refined with riding coordinates: N3(H3), N2(H2), C7(H7), C12(H12), C2(H2A), C5(H5), C9(H9), C15(H15), C4(H4), C10(H10), C18(H18), C3(H3A), C11(H11), C20(H20), C19(H19) ; _shelx_res_file ; TITL test_0m_a.res in P2(1)/n test_0m_a.res created by SHELXL-2019/1 at 12:20:26 on 17-Nov-2023 CELL 0.71073 3.9684 19.4601 25.0841 90 91.789 90 ZERR 4 0.0023 0.0106 0.0134 0 0.02 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cl N S UNIT 88 60 8 12 4 L.S. 20 PLAN 5 TEMP 23.85 CONF BOND $H MORE -1 fmap 2 acta OMIT -3 50 REM REM REM WGHT 0.083000 1.982700 FVAR 0.54340 S1 5 0.910194 0.397521 0.540365 11.00000 0.06636 0.04957 = 0.03046 -0.00354 -0.00909 -0.00505 CL1 3 0.932192 0.216797 0.386366 11.00000 0.08199 0.06427 = 0.03383 -0.00630 0.01294 -0.00421 CL2 3 0.898053 0.066340 0.432349 11.00000 0.10885 0.05207 = 0.07712 -0.01240 0.00549 0.01958 N1 4 0.646580 0.430231 0.391612 11.00000 0.05548 0.04650 = 0.02001 -0.00288 -0.00558 -0.00757 N3 4 0.670792 0.324528 0.455821 11.00000 0.06680 0.03666 = 0.02587 0.00075 -0.00722 -0.00719 AFIX 43 H3 2 0.601353 0.326440 0.423033 11.00000 -1.20000 AFIX 0 N2 4 0.742675 0.439662 0.444393 11.00000 0.07543 0.03621 = 0.02654 -0.00140 -0.01178 -0.00489 AFIX 43 H2 2 0.788430 0.480298 0.455988 11.00000 -1.20000 AFIX 0 C8 1 0.295724 0.543539 0.230003 11.00000 0.03007 0.03700 = 0.03362 0.00562 0.00042 -0.00836 C13 1 0.393740 0.542419 0.284672 11.00000 0.03871 0.03289 = 0.02783 0.00268 0.00355 -0.00524 C1 1 0.648951 0.427952 0.271710 11.00000 0.02946 0.02946 = 0.03492 0.00709 0.00488 -0.00723 C14 1 0.567222 0.483544 0.305696 11.00000 0.03634 0.03789 = 0.02511 0.00342 -0.00032 -0.00993 C7 1 0.371481 0.487180 0.197970 11.00000 0.04589 0.04776 = 0.02857 0.00416 -0.00142 -0.00929 AFIX 43 H7 2 0.300231 0.487854 0.162300 11.00000 -1.20000 AFIX 0 C6 1 0.549433 0.429886 0.217137 11.00000 0.03845 0.03655 = 0.03550 0.00052 0.00804 -0.01291 C17 1 0.670857 0.258127 0.479331 11.00000 0.04230 0.03959 = 0.03072 0.00046 0.00096 -0.00861 C12 1 0.307074 0.599796 0.316068 11.00000 0.04503 0.04368 = 0.03966 -0.00052 0.00048 -0.00001 AFIX 43 H12 2 0.364952 0.599900 0.352282 11.00000 -1.20000 AFIX 0 C2 1 0.849967 0.369596 0.288649 11.00000 0.04506 0.04179 = 0.03501 0.00311 0.00770 -0.00085 AFIX 43 H2A 2 0.927220 0.367133 0.323984 11.00000 -1.20000 AFIX 0 C5 1 0.631126 0.374398 0.183157 11.00000 0.04695 0.06235 = 0.03178 -0.01566 0.01453 -0.01528 AFIX 43 H5 2 0.555241 0.375185 0.147708 11.00000 -1.20000 AFIX 0 C9 1 0.118836 0.601773 0.209170 11.00000 0.04129 0.05681 = 0.04806 0.01203 -0.00675 -0.00399 AFIX 43 H9 2 0.051617 0.602680 0.173326 11.00000 -1.20000 AFIX 0 C15 1 0.656452 0.483852 0.362222 11.00000 0.05044 0.03581 = 0.03412 0.00299 -0.00469 0.00016 AFIX 43 H15 2 0.724248 0.525119 0.377877 11.00000 -1.20000 AFIX 0 C16 1 0.765545 0.385408 0.478112 11.00000 0.03682 0.04402 = 0.02804 -0.00787 0.00362 -0.00324 C4 1 0.818396 0.319933 0.201296 11.00000 0.05005 0.03346 = 0.06478 -0.01460 0.02477 -0.00671 AFIX 43 H4 2 0.871783 0.284206 0.178428 11.00000 -1.20000 AFIX 0 C10 1 0.047161 0.655844 0.240830 11.00000 0.05341 0.04185 = 0.06725 0.01665 -0.00353 -0.00321 AFIX 43 H10 2 -0.065481 0.693812 0.226499 11.00000 -1.20000 AFIX 0 C18 1 0.551904 0.245652 0.530075 11.00000 0.05562 0.05925 = 0.03621 -0.00320 0.01314 -0.00204 AFIX 43 H18 2 0.474244 0.281963 0.550434 11.00000 -1.20000 AFIX 0 C22 1 0.785851 0.202036 0.448919 11.00000 0.04396 0.04678 = 0.03124 -0.00397 0.00076 0.00135 C3 1 0.929259 0.318607 0.254948 11.00000 0.05615 0.04502 = 0.04827 0.00332 0.01703 -0.00042 AFIX 43 H3A 2 1.059587 0.281937 0.267448 11.00000 -1.20000 AFIX 0 C11 1 0.140939 0.654846 0.294491 11.00000 0.05152 0.04237 = 0.07283 0.00406 0.00700 0.00323 AFIX 43 H11 2 0.089904 0.692139 0.315973 11.00000 -1.20000 AFIX 0 C21 1 0.771986 0.136225 0.469934 11.00000 0.05697 0.04033 = 0.04461 -0.00860 -0.00246 0.00440 C20 1 0.656772 0.124923 0.520049 11.00000 0.07175 0.04754 = 0.05010 0.00664 0.00172 -0.00322 AFIX 43 H20 2 0.651072 0.080555 0.533769 11.00000 -1.20000 AFIX 0 C19 1 0.548590 0.179851 0.550290 11.00000 0.07321 0.05697 = 0.04422 0.01195 0.01185 -0.01252 AFIX 43 H19 2 0.473145 0.172200 0.584516 11.00000 -1.20000 AFIX 0 HKLF 4 REM test_0m_a.res in P2(1)/n REM wR2 = 0.2131, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0778 for 1805 Fo > 4sig(Fo) and 0.1621 for all 3411 data REM 253 parameters refined using 0 restraints END WGHT 0.0830 1.9764 REM Highest difference peak 0.642, deepest hole -0.342, 1-sigma level 0.084 Q1 1 0.5637 0.2224 0.3856 11.00000 0.05 0.64 Q2 1 1.2845 0.2160 0.3901 11.00000 0.05 0.55 Q3 1 0.5588 0.3993 0.5377 11.00000 0.05 0.50 Q4 1 1.2565 0.0745 0.4366 11.00000 0.05 0.46 Q5 1 1.2232 0.3946 0.5453 11.00000 0.05 0.44 ; _shelx_res_checksum 32414 _shelx_hkl_file ; 1 0 0 -15.70 8.40 1 0 0 -7.00 7.40 1 0 0 2.70 7.30 -1 0 0 -2.40 7.10 -1 0 0 2.20 6.70 -1 0 0 4.30 6.60 -2 0 0 13.00 14.10 2 0 0 2.70 20.70 2 0 0 2.20 11.40 -2 0 0 -4.00 12.60 -2 0 0 -0.20 12.00 2 0 0 13.30 18.10 3 0 0 7.90 18.50 -3 0 0 31.70 22.80 -3 0 0 25.90 23.60 -3 0 0 41.50 25.70 -4 0 0 108.99 43.30 4 0 0 85.59 32.90 -4 0 0 129.29 43.90 -1 -1 0 1225.08 169.18 1 -1 0 1340.77 169.48 -1 -1 0 1313.97 169.38 1 -1 0 1268.67 169.48 1 -1 0 1247.08 169.38 -1 -1 0 1130.39 169.28 -1 1 0 1338.47 169.38 -1 1 0 1281.67 169.38 -1 1 0 1196.08 169.28 1 1 0 1218.28 169.38 1 1 0 1334.47 169.38 1 1 0 1174.28 169.38 -2 -1 0 297.27 42.20 2 -1 0 190.58 42.60 2 -1 0 283.17 43.20 -2 -1 0 349.37 43.60 2 -1 0 266.07 42.10 -2 -1 0 249.38 41.70 2 1 0 289.97 43.30 2 1 0 329.67 45.70 -2 1 0 262.27 41.90 2 1 0 271.77 41.00 -2 1 0 365.06 43.80 -2 1 0 232.48 41.70 -3 -1 0 97.49 28.40 3 -1 0 148.09 26.90 -3 -1 0 148.39 31.10 -3 -1 0 97.29 31.30 3 1 0 136.99 27.10 -3 1 0 55.99 28.90 -3 1 0 127.39 29.80 -3 1 0 182.38 29.50 -4 -1 0 16.60 43.90 -4 -1 0 26.40 42.40 4 -1 0 51.99 29.80 4 1 0 26.50 31.40 -4 1 0 -34.10 44.70 -4 1 0 77.69 42.50 0 -2 0 523.45 68.69 0 -2 0 524.65 68.79 0 -2 0 494.45 68.79 0 2 0 501.25 68.79 1 -2 0 4892.41 679.63 -1 -2 0 5342.77 679.73 1 -2 0 5057.19 679.73 -1 -2 0 4765.92 679.63 1 -2 0 4980.40 679.83 -1 -2 0 5269.07 679.53 -1 2 0 4697.53 679.73 -1 2 0 4961.90 679.73 -1 2 0 5237.48 679.73 1 2 0 4967.30 679.63 1 2 0 5252.57 679.73 1 2 0 5112.69 679.53 1 2 0 5203.38 679.53 2 -2 0 141.39 28.20 -2 -2 0 150.88 25.90 -2 -2 0 193.98 26.00 2 -2 0 143.79 25.50 2 -2 0 148.89 28.20 -2 -2 0 186.88 26.00 -2 2 0 164.58 27.10 -2 2 0 161.18 26.30 2 2 0 153.58 29.20 2 2 0 151.18 27.70 -2 2 0 77.49 25.80 2 2 0 148.29 24.40 -3 -2 0 126.59 27.70 -3 -2 0 116.49 31.10 3 -2 0 52.89 27.00 -3 -2 0 238.78 30.60 -3 2 0 158.18 31.90 -3 2 0 122.09 31.40 3 2 0 133.09 27.50 -3 2 0 34.00 28.00 -4 -2 0 86.99 43.50 4 -2 0 44.80 30.20 4 2 0 65.29 33.60 -4 2 0 -22.80 40.10 -4 2 0 44.70 46.40 0 -3 0 4.80 2.80 0 -3 0 2.90 2.50 0 -3 0 0.00 1.70 0 3 0 3.40 1.80 0 3 0 0.20 2.60 0 3 0 1.30 2.10 1 -3 0 3888.51 508.75 1 -3 0 3763.52 508.85 1 -3 0 3540.55 508.65 -1 -3 0 3999.60 508.45 -1 -3 0 3921.41 508.65 1 3 0 3851.21 508.45 -1 3 0 4040.90 508.75 1 3 0 3767.42 508.55 -1 3 0 3670.83 508.75 1 3 0 3794.22 508.75 1 3 0 3559.14 508.55 1 3 0 3802.72 508.85 1 3 0 3539.85 508.65 -1 3 0 3832.72 508.85 -2 -3 0 29.60 13.80 2 -3 0 15.60 18.60 2 -3 0 4.70 12.30 -2 -3 0 16.40 15.70 -2 -3 0 -15.40 12.50 2 -3 0 1.50 19.50 2 3 0 -3.60 11.30 2 3 0 -9.10 17.90 2 3 0 6.80 19.20 -2 3 0 -16.90 14.30 -2 3 0 28.90 14.00 -2 3 0 -4.60 14.60 -3 -3 0 39.10 25.20 3 -3 0 67.39 22.60 -3 -3 0 79.29 28.40 3 3 0 61.89 21.80 -3 3 0 34.10 24.30 -3 3 0 86.59 26.80 -3 3 0 55.59 27.80 -4 -3 0 38.10 35.90 4 -3 0 29.00 34.30 -4 3 0 -21.00 38.90 -4 3 0 1.10 45.90 4 3 0 -0.60 31.50 4 3 0 -12.80 32.10 0 -4 0 2380.26 291.67 0 -4 0 2011.40 291.67 0 -4 0 2150.18 291.57 0 4 0 2210.98 291.67 0 4 0 2188.88 291.67 0 4 0 2083.59 291.67 -1 -4 0 1115.89 138.59 1 -4 0 983.60 139.79 -1 -4 0 864.91 138.99 1 -4 0 1045.20 139.19 1 4 0 1014.90 138.89 -1 4 0 1019.30 139.09 1 4 0 1039.40 138.69 -1 4 0 937.61 138.99 1 4 0 1113.89 139.29 -1 4 0 985.70 138.99 1 4 0 1046.50 138.69 1 4 0 1148.09 138.59 -2 -4 0 93.69 20.40 2 -4 0 100.69 22.90 2 -4 0 129.19 25.10 -2 -4 0 124.89 21.40 2 -4 0 82.89 19.50 2 4 0 86.19 19.90 2 4 0 93.59 25.40 -2 4 0 80.49 22.00 2 4 0 104.39 18.80 -2 4 0 125.89 22.70 2 4 0 86.19 19.50 2 4 0 135.89 26.10 -2 4 0 100.39 20.50 -3 -4 0 22.30 24.80 3 -4 0 -1.30 19.60 -3 4 0 8.10 30.00 -3 4 0 -11.30 23.40 3 4 0 39.80 23.20 -3 4 0 36.80 26.10 3 4 0 12.50 18.90 3 4 0 14.30 20.50 -4 -4 0 21.50 41.80 4 -4 0 18.50 30.60 4 4 0 30.50 29.50 4 4 0 -16.70 39.90 4 4 0 9.00 30.80 -4 4 0 25.60 40.90 -4 4 0 61.79 42.60 0 -5 0 2.90 3.80 0 -5 0 4.60 2.50 0 -5 0 5.50 4.50 0 5 0 9.80 4.50 0 5 0 3.90 3.40 0 5 0 1.50 3.10 -1 -5 0 602.24 81.89 -1 -5 0 563.14 80.89 1 -5 0 582.74 81.39 1 -5 0 509.25 81.99 1 -5 0 617.44 81.49 -1 5 0 543.25 81.39 1 5 0 603.74 80.89 1 5 0 644.74 80.69 1 5 0 631.74 80.49 1 5 0 589.34 80.59 1 5 0 673.13 82.19 -1 5 0 582.94 81.19 -1 5 0 570.24 81.29 2 -5 0 264.97 39.50 2 -5 0 270.37 41.70 -2 -5 0 268.77 39.40 2 -5 0 251.87 40.20 2 5 0 228.08 38.70 -2 5 0 225.98 39.80 2 5 0 226.58 42.90 2 5 0 218.18 38.70 -2 5 0 265.77 40.60 2 5 0 269.37 38.80 2 5 0 287.07 40.80 2 5 0 300.57 41.20 -2 5 0 268.17 40.50 3 -5 0 45.10 22.60 -3 -5 0 45.80 23.20 -3 5 0 -17.60 25.00 3 5 0 29.40 18.80 -3 5 0 -21.50 30.60 -3 5 0 40.80 25.70 3 5 0 20.80 21.40 3 5 0 31.80 22.10 -4 -5 0 8.30 42.90 4 -5 0 27.20 30.50 4 5 0 59.39 40.80 4 5 0 25.50 32.20 -4 5 0 -36.30 47.00 -4 5 0 15.20 49.00 4 5 0 2.50 29.00 0 -6 0 1562.64 196.68 0 -6 0 1471.35 196.88 0 -6 0 1476.55 196.78 0 -6 0 1448.96 196.78 0 6 0 1502.65 196.78 0 6 0 1419.76 196.78 0 6 0 1353.66 196.78 1 -6 0 157.28 22.40 1 -6 0 146.89 22.80 -1 -6 0 165.88 24.00 -1 -6 0 159.58 22.20 1 -6 0 130.69 24.80 -1 6 0 107.29 22.50 1 6 0 149.39 20.90 1 6 0 154.48 20.50 -1 6 0 91.99 22.50 1 6 0 143.39 21.50 1 6 0 153.78 21.00 2 -6 0 -8.90 15.20 2 -6 0 -0.80 18.10 2 6 0 32.30 14.30 2 6 0 -11.70 16.60 2 6 0 33.40 22.80 -2 6 0 -5.40 16.90 2 6 0 19.00 19.80 2 6 0 -6.40 11.80 2 6 0 30.90 11.40 -2 6 0 21.10 14.60 -2 6 0 10.40 15.60 3 -6 0 146.69 35.50 -3 -6 0 198.18 36.20 -3 6 0 162.08 37.10 3 6 0 189.68 34.70 3 6 0 158.08 32.20 -3 6 0 217.38 37.20 3 6 0 154.08 31.00 -3 6 0 159.98 37.70 4 -6 0 16.10 34.10 -4 -6 0 -51.09 38.20 -4 6 0 -22.80 40.80 4 6 0 30.20 31.80 4 6 0 40.80 35.00 -4 6 0 -2.40 52.29 4 6 0 -18.60 33.40 0 -7 0 5.30 6.60 0 -7 0 -7.20 3.70 0 -7 0 8.40 5.50 0 -7 0 13.40 5.90 0 7 0 1.10 6.10 0 7 0 5.70 4.60 0 7 0 0.90 4.80 1 -7 0 1687.13 228.18 1 -7 0 1678.93 228.18 1 7 0 1775.92 227.28 1 7 0 1675.33 227.58 -1 7 0 1530.65 228.18 1 7 0 1635.14 227.28 -1 7 0 1679.43 228.28 -1 7 0 1900.21 228.58 1 7 0 1675.93 227.88 2 -7 0 36.20 18.90 2 7 0 66.89 16.20 2 7 0 80.69 15.60 2 7 0 98.89 16.20 2 7 0 45.40 19.70 2 7 0 80.99 25.70 -2 7 0 80.19 21.30 -2 7 0 19.00 17.40 -2 7 0 70.09 21.00 3 -7 0 -14.50 21.50 -3 7 0 2.70 24.40 3 7 0 -8.00 24.00 -3 7 0 -2.90 25.70 -3 7 0 53.39 29.40 3 7 0 -8.30 21.80 3 7 0 2.90 19.70 4 -7 0 70.19 31.90 4 7 0 -18.60 34.60 -4 7 0 60.59 56.09 4 7 0 16.50 39.50 -4 7 0 -20.70 43.10 0 -8 0 410.26 55.09 0 -8 0 384.26 54.99 0 -8 0 446.96 54.49 0 -8 0 408.16 55.19 0 8 0 361.96 54.69 0 8 0 369.76 54.79 0 8 0 424.56 54.99 1 -8 0 46.80 10.80 -1 -8 0 20.70 11.20 -1 -8 0 29.70 13.10 1 -8 0 56.59 13.00 1 -8 0 52.09 12.00 -1 8 0 47.30 10.50 -1 8 0 39.30 12.60 -1 8 0 44.90 12.50 1 8 0 20.60 6.70 1 8 0 22.10 8.20 2 -8 0 -3.80 18.70 2 8 0 9.20 11.70 2 8 0 -25.40 15.60 2 8 0 4.50 23.80 -2 8 0 1.60 19.30 -2 8 0 -9.00 20.10 -2 8 0 -1.80 17.10 2 8 0 9.90 12.00 2 8 0 -7.10 13.30 3 -8 0 59.49 24.20 -3 8 0 20.40 33.30 3 8 0 4.00 22.80 -3 8 0 11.50 28.00 -3 8 0 44.80 26.70 3 8 0 74.89 25.30 3 8 0 29.30 21.40 4 -8 0 41.10 33.80 -4 8 0 -27.90 48.00 4 8 0 12.90 34.70 -4 8 0 35.30 55.59 4 8 0 31.20 41.40 0 -9 0 9.20 7.90 0 -9 0 2.60 8.00 0 -9 0 0.20 5.20 0 -9 0 -4.00 8.60 0 9 0 -19.10 6.20 0 9 0 -1.80 6.00 1 -9 0 29.10 14.20 1 -9 0 18.00 14.60 -1 -9 0 12.70 11.10 1 -9 0 28.90 13.40 -1 -9 0 45.00 15.30 -1 9 0 52.29 12.80 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33.10 2 -3 -24 61.59 20.00 2 -3 -24 43.00 23.20 2 3 -24 50.09 23.70 2 3 -24 18.20 24.30 1 -3 -24 26.00 22.00 1 3 -24 56.69 15.80 1 3 -24 32.80 22.70 0 -3 -24 42.40 19.80 0 3 -24 -2.60 20.40 0 3 -24 -8.40 16.10 -1 -3 -24 -20.20 26.20 -1 3 -24 9.00 24.90 -1 3 -24 -3.90 19.20 -2 -3 -24 227.08 48.90 -2 3 -24 178.88 48.10 2 -4 -24 49.90 25.00 2 -4 -24 72.19 26.50 2 4 -24 111.09 25.20 2 4 -24 70.59 27.50 1 -4 -24 96.09 21.80 1 4 -24 48.50 19.20 1 4 -24 57.39 23.60 0 -4 -24 72.49 26.30 0 4 -24 83.09 23.70 0 4 -24 82.89 20.70 -1 -4 -24 -8.10 23.10 -1 4 -24 5.50 20.20 -1 4 -24 -31.40 28.70 -2 -4 -24 14.50 35.40 -2 4 -24 2.10 39.20 2 -5 -24 -6.70 19.10 2 5 -24 42.80 24.70 2 5 -24 19.60 25.20 1 -5 -24 70.59 19.90 1 5 -24 15.10 24.60 1 5 -24 42.50 17.50 0 -5 -24 3.50 18.90 0 5 -24 59.39 27.30 0 5 -24 9.60 15.40 -1 -5 -24 79.59 26.20 -1 5 -24 64.69 25.60 -1 5 -24 91.49 33.40 -2 -5 -24 40.70 39.40 -2 5 -24 4.90 29.50 -2 5 -24 35.10 38.60 2 -6 -24 4.50 20.80 2 6 -24 14.90 24.10 2 6 -24 29.90 26.00 1 -6 -24 108.59 24.90 1 6 -24 80.29 22.40 1 6 -24 109.59 26.10 0 -6 -24 40.70 21.00 0 6 -24 19.00 19.40 0 6 -24 22.50 24.10 -1 -6 -24 18.30 28.50 -1 6 -24 -5.40 20.60 -1 6 -24 15.80 27.00 -2 -6 -24 89.19 35.60 -2 6 -24 12.00 37.40 -2 6 -24 14.70 34.00 2 -7 -24 24.80 22.50 2 7 -24 -8.60 27.10 2 7 -24 -8.50 23.00 1 -7 -24 70.49 22.30 1 7 -24 65.29 23.70 1 7 -24 31.60 21.50 0 -7 -24 4.90 20.90 0 7 -24 -13.20 17.20 0 7 -24 10.80 27.90 -1 -7 -24 26.50 26.10 -1 7 -24 11.20 35.20 -1 7 -24 2.10 22.10 -2 -7 -24 327.17 54.89 -2 7 -24 272.77 59.09 -2 7 -24 214.08 47.40 2 -8 -24 -2.80 27.10 2 8 -24 -21.40 22.60 2 8 -24 -0.20 26.70 1 -8 -24 84.89 27.70 1 8 -24 31.40 28.30 1 8 -24 90.19 21.60 0 -8 -24 14.70 23.90 0 8 -24 -9.00 19.10 0 8 -24 52.19 28.00 -1 -8 -24 102.39 31.10 -1 8 -24 15.00 37.00 -1 8 -24 69.59 24.90 -2 -8 -24 -21.70 40.10 -2 8 -24 -28.80 32.00 -2 8 -24 1.80 41.70 2 -9 -24 8.20 24.30 2 9 -24 -4.70 22.40 2 9 -24 -12.70 28.50 1 -9 -24 20.90 23.40 1 9 -24 5.10 20.10 1 9 -24 2.20 27.20 0 -9 -24 39.00 22.40 0 9 -24 -0.90 22.30 0 9 -24 6.50 31.70 -1 -9 -24 66.39 32.20 -1 9 -24 51.79 29.40 -1 9 -24 60.09 32.90 -2 -9 -24 16.00 42.00 -2 9 -24 -5.40 40.40 -2 9 -24 -5.00 43.90 2 -10 -24 -32.30 29.60 2 10 -24 9.70 30.30 2 10 -24 16.90 28.10 1 -10 -24 9.90 26.10 1 10 -24 82.09 30.70 1 10 -24 35.40 22.10 0 -10 -24 159.68 29.50 0 10 -24 53.59 24.10 0 10 -24 60.79 35.40 -1 -10 -24 21.30 30.10 -1 10 -24 0.10 38.40 -1 10 -24 5.20 29.30 1 -11 -24 28.50 27.20 1 11 -24 -11.40 20.20 1 11 -24 21.30 31.70 0 -11 -24 16.40 26.30 0 11 -24 21.30 23.50 0 11 -24 23.50 31.00 -1 -11 -24 49.00 31.90 -1 11 -24 66.89 40.60 -1 11 -24 17.60 27.70 1 -12 -24 71.49 30.80 1 12 -24 85.59 37.40 1 12 -24 81.29 25.20 0 -12 -24 10.50 26.10 0 12 -24 94.09 37.60 0 12 -24 -0.10 23.90 -1 12 -24 23.60 38.00 -1 12 -24 -26.20 28.40 1 -13 -24 -25.50 24.10 1 13 -24 12.90 34.10 1 13 -24 -26.10 23.20 0 -13 -24 87.09 30.20 0 13 -24 58.39 41.00 0 13 -24 71.79 27.50 2 0 -25 -6.70 21.40 2 0 -25 -24.10 23.80 1 0 -25 22.00 22.00 1 0 -25 17.90 14.70 0 0 -25 -10.10 15.80 0 0 -25 -16.60 20.80 -1 0 -25 155.58 34.30 -2 0 -25 -10.00 39.60 2 -1 -25 134.19 28.70 2 -1 -25 95.69 30.10 2 1 -25 137.19 29.00 2 1 -25 126.39 28.10 1 -1 -25 50.59 16.70 1 -1 -25 76.29 22.10 1 1 -25 38.80 17.90 1 1 -25 81.89 23.10 0 -1 -25 25.00 22.30 0 1 -25 5.60 16.60 0 1 -25 21.80 21.50 -1 -1 -25 29.80 26.00 -1 1 -25 22.70 26.10 -2 -1 -25 22.00 32.60 -2 1 -25 61.69 37.30 2 -2 -25 -14.60 23.00 2 -2 -25 19.10 24.40 2 2 -25 -19.70 22.40 2 2 -25 49.00 21.60 1 -2 -25 -12.10 22.60 1 -2 -25 24.80 19.80 1 2 -25 4.10 20.00 1 2 -25 13.70 16.50 0 -2 -25 10.60 23.70 0 2 -25 73.29 22.30 0 2 -25 15.90 17.80 -1 -2 -25 44.50 29.40 -1 2 -25 -3.90 26.50 -2 -2 -25 -3.60 33.90 -2 2 -25 16.80 42.10 2 -3 -25 50.59 24.90 2 -3 -25 42.90 23.20 2 3 -25 -19.60 24.00 2 3 -25 39.70 24.00 1 -3 -25 27.50 23.90 1 3 -25 26.10 16.30 1 3 -25 52.29 23.00 0 -3 -25 49.50 21.30 0 3 -25 11.20 17.50 0 3 -25 37.60 24.90 -1 -3 -25 26.40 26.20 -1 3 -25 32.10 22.80 -1 3 -25 4.80 30.20 -2 -3 -25 14.30 41.20 -2 3 -25 28.00 36.50 2 -4 -25 135.19 28.80 2 4 -25 191.18 31.80 2 4 -25 81.49 30.90 1 -4 -25 -3.50 20.90 1 4 -25 3.90 22.90 1 4 -25 0.80 18.50 0 -4 -25 33.30 24.30 0 4 -25 98.29 26.50 0 4 -25 22.70 19.80 -1 -4 -25 11.40 24.60 -1 4 -25 -14.50 21.70 -1 4 -25 4.50 27.60 -2 -4 -25 11.70 40.30 -2 4 -25 -18.60 37.30 2 -5 -25 21.30 23.10 2 5 -25 24.50 25.00 2 5 -25 15.20 27.00 1 -5 -25 10.60 22.50 1 5 -25 -12.80 18.80 1 5 -25 50.79 25.20 0 -5 -25 80.99 27.60 0 5 -25 90.29 33.20 0 5 -25 150.88 25.20 -1 -5 -25 30.40 26.90 -1 5 -25 33.30 32.40 -1 5 -25 28.60 24.20 -2 -5 -25 44.80 41.10 -2 5 -25 13.70 35.20 2 -6 -25 1.30 23.30 2 6 -25 15.00 24.30 2 6 -25 50.99 26.90 1 -6 -25 -11.10 19.90 1 6 -25 17.60 17.40 1 6 -25 -3.50 23.00 0 -6 -25 24.20 22.60 0 6 -25 37.60 19.80 0 6 -25 58.49 27.40 -1 -6 -25 73.69 34.30 -1 6 -25 76.59 27.60 -1 6 -25 101.09 37.70 -2 -6 -25 10.80 36.90 -2 6 -25 1.10 35.30 -2 6 -25 40.60 42.80 2 -7 -25 31.90 24.70 2 7 -25 55.99 26.60 2 7 -25 58.29 29.50 1 -7 -25 132.59 23.70 1 7 -25 6.40 25.80 1 7 -25 1.90 20.90 0 -7 -25 59.89 21.90 0 7 -25 -14.30 29.20 0 7 -25 -7.10 21.50 -1 -7 -25 -9.40 29.60 -1 7 -25 16.50 25.40 -1 7 -25 6.30 36.30 -2 -7 -25 2.10 36.60 -2 7 -25 -31.90 35.50 -2 7 -25 14.70 40.60 2 -8 -25 9.20 24.00 2 8 -25 -6.80 27.40 2 8 -25 33.70 30.60 1 -8 -25 84.99 26.80 1 8 -25 23.00 20.10 1 8 -25 98.79 28.20 0 -8 -25 71.29 27.60 0 8 -25 20.40 28.40 0 8 -25 2.00 19.20 -1 -8 -25 18.40 31.50 -1 8 -25 -29.90 37.50 -1 8 -25 4.70 24.90 1 -9 -25 32.60 23.80 1 9 -25 8.00 29.60 1 9 -25 46.40 21.50 0 -9 -25 40.30 24.40 0 9 -25 -4.90 20.60 0 9 -25 28.90 30.40 -1 -9 -25 -10.80 33.00 -1 9 -25 29.60 34.20 -1 9 -25 20.60 29.30 1 -10 -25 73.99 27.90 1 10 -25 51.29 26.20 1 10 -25 -15.30 31.60 0 -10 -25 -10.50 24.00 0 10 -25 -2.60 26.20 0 10 -25 38.60 32.10 -1 -10 -25 11.80 31.90 -1 10 -25 1.90 27.00 -1 10 -25 30.10 41.50 1 -11 -25 55.79 27.60 1 11 -25 -4.00 35.50 1 11 -25 -5.30 21.20 0 -11 -25 107.19 28.70 0 11 -25 76.29 31.90 0 11 -25 120.39 42.00 -1 -11 -25 -2.10 32.90 -1 11 -25 71.29 37.10 -1 11 -25 -30.70 29.50 1 -12 -25 49.40 29.10 1 12 -25 6.00 38.90 1 12 -25 -5.10 24.40 0 -12 -25 40.00 29.90 0 12 -25 43.70 38.60 0 12 -25 1.00 28.90 2 0 -26 5.00 25.50 2 0 -26 -11.70 24.10 1 0 -26 7.60 17.10 1 0 -26 -4.20 21.80 0 0 -26 45.30 27.90 -1 0 -26 -0.50 30.70 -2 0 -26 176.48 48.70 2 -1 -26 33.70 23.80 2 -1 -26 10.20 22.20 2 1 -26 45.70 25.10 2 1 -26 40.90 27.80 1 -1 -26 0.70 17.10 1 -1 -26 32.40 21.20 1 1 -26 14.30 16.20 1 1 -26 -4.80 22.40 0 -1 -26 -32.90 25.00 0 1 -26 -16.30 18.80 0 1 -26 18.80 22.20 -1 -1 -26 8.50 28.00 -1 1 -26 38.90 31.70 -2 -1 -26 6.00 37.10 -2 1 -26 86.89 39.20 2 -2 -26 -17.10 23.20 2 -2 -26 11.70 23.30 2 2 -26 -5.50 25.70 2 2 -26 49.00 24.90 1 -2 -26 28.80 22.50 1 2 -26 -11.20 16.70 1 2 -26 -8.60 26.40 0 -2 -26 24.10 26.60 0 2 -26 1.70 18.10 0 2 -26 -12.90 23.60 -1 -2 -26 13.60 33.20 -1 2 -26 30.00 33.70 -2 -2 -26 33.60 39.00 -2 2 -26 -0.90 43.90 2 -3 -26 10.30 22.70 2 3 -26 14.40 22.10 2 3 -26 30.80 25.80 1 -3 -26 20.30 21.00 1 3 -26 34.20 24.50 1 3 -26 34.60 17.50 0 -3 -26 19.30 23.80 0 3 -26 44.80 25.10 0 3 -26 5.90 17.20 -1 -3 -26 45.60 28.90 -1 3 -26 -10.10 28.00 -2 -3 -26 6.90 44.70 -2 3 -26 22.00 38.40 2 -4 -26 2.70 25.40 2 4 -26 22.00 25.90 2 4 -26 15.30 24.50 1 -4 -26 24.00 23.10 1 4 -26 8.20 16.60 1 4 -26 1.70 23.20 0 -4 -26 7.80 26.20 0 4 -26 -12.60 26.80 0 4 -26 8.60 19.40 -1 -4 -26 56.29 29.70 -1 4 -26 20.80 34.70 -1 4 -26 24.80 24.70 -2 -4 -26 -20.40 41.10 -2 4 -26 -4.10 38.50 2 -5 -26 21.40 26.60 2 5 -26 -4.60 29.80 2 5 -26 -0.60 26.50 1 -5 -26 141.69 30.00 1 5 -26 73.79 26.00 1 5 -26 113.89 32.60 0 -5 -26 11.80 22.70 0 5 -26 17.40 20.50 0 5 -26 24.30 28.30 -1 -5 -26 108.19 33.10 -1 5 -26 102.99 35.50 -1 5 -26 87.39 28.70 -2 -5 -26 72.19 45.40 -2 5 -26 -39.20 38.40 2 -6 -26 17.70 26.00 2 6 -26 -1.00 22.70 2 6 -26 44.30 27.40 1 -6 -26 95.79 23.00 1 6 -26 21.30 26.40 1 6 -26 43.40 22.80 0 -6 -26 13.30 23.50 0 6 -26 4.70 18.10 0 6 -26 7.30 27.80 -1 -6 -26 -34.00 33.30 -1 6 -26 33.40 26.10 -1 6 -26 -34.70 36.50 2 -7 -26 -1.60 26.60 2 7 -26 13.40 31.20 2 7 -26 -0.60 24.60 1 -7 -26 12.70 26.90 1 7 -26 8.90 29.00 1 7 -26 28.30 19.50 0 -7 -26 -9.40 27.80 0 7 -26 12.30 31.20 0 7 -26 -10.50 22.70 -1 -7 -26 37.00 29.50 -1 7 -26 14.20 27.80 -1 7 -26 30.90 37.50 1 -8 -26 2.60 27.40 1 8 -26 21.30 31.00 1 8 -26 -0.20 24.30 0 -8 -26 -13.80 27.60 0 8 -26 27.80 30.90 0 8 -26 7.20 24.60 -1 -8 -26 -5.50 33.60 -1 8 -26 22.10 27.10 -1 8 -26 43.70 41.80 1 -9 -26 -5.70 25.60 1 9 -26 26.10 32.10 1 9 -26 7.10 22.00 0 -9 -26 -9.20 30.00 0 9 -26 2.90 33.90 0 9 -26 21.10 26.20 -1 -9 -26 -5.40 35.90 -1 9 -26 -19.00 33.00 -1 9 -26 1.90 36.20 1 -10 -26 19.40 26.30 1 10 -26 8.20 36.40 1 10 -26 46.00 27.20 0 -10 -26 112.99 32.90 0 10 -26 25.60 38.90 0 10 -26 39.00 26.30 -1 -10 -26 -7.40 34.90 -1 10 -26 -15.90 37.40 -1 10 -26 21.70 30.40 0 -11 -26 57.49 31.10 0 11 -26 26.80 39.40 0 11 -26 0.80 28.80 2 0 -27 -0.10 26.40 2 0 -27 48.50 25.20 1 0 -27 35.00 20.30 1 0 -27 19.10 24.40 0 0 -27 24.40 24.50 -1 0 -27 188.08 45.00 2 -1 -27 -1.50 21.90 2 -1 -27 12.50 24.00 2 1 -27 41.10 28.80 2 1 -27 3.00 24.70 1 -1 -27 1.80 23.30 1 1 -27 22.10 24.50 1 1 -27 38.70 20.00 0 -1 -27 7.60 24.40 0 1 -27 -29.20 28.90 -1 -1 -27 -24.60 30.10 -1 1 -27 82.09 35.10 2 -2 -27 -2.20 24.90 2 2 -27 -23.80 25.50 2 2 -27 4.20 23.40 1 -2 -27 151.28 28.40 1 2 -27 77.89 21.40 1 2 -27 107.49 29.80 0 -2 -27 10.90 29.50 0 2 -27 18.30 25.40 0 2 -27 9.20 25.60 -1 -2 -27 33.90 34.40 -1 2 -27 -0.50 35.90 2 -3 -27 13.00 28.70 2 3 -27 36.60 28.80 2 3 -27 77.49 27.60 1 -3 -27 45.70 24.00 1 3 -27 78.19 30.70 1 3 -27 49.90 20.40 0 -3 -27 3.50 24.50 0 3 -27 -7.70 21.10 0 3 -27 -14.80 29.40 -1 -3 -27 18.40 30.20 -1 3 -27 18.30 37.90 2 -4 -27 -9.00 23.90 2 4 -27 -25.40 22.90 2 4 -27 41.30 27.90 1 -4 -27 12.70 25.60 1 4 -27 33.80 30.20 1 4 -27 1.30 19.30 0 -4 -27 29.30 29.70 0 4 -27 11.10 20.30 0 4 -27 -7.90 28.70 -1 -4 -27 14.10 30.00 -1 4 -27 0.30 33.60 1 -5 -27 13.70 22.40 1 5 -27 24.50 30.00 1 5 -27 -9.40 18.40 0 -5 -27 125.79 32.10 0 5 -27 69.69 32.40 0 5 -27 46.90 23.90 -1 -5 -27 6.70 31.20 -1 5 -27 9.50 27.70 -1 5 -27 -1.60 36.30 1 -6 -27 28.70 23.60 1 6 -27 34.00 20.30 1 6 -27 31.50 28.80 0 -6 -27 16.70 30.00 0 6 -27 -28.40 22.30 0 6 -27 -16.60 29.80 -1 -6 -27 62.99 38.20 -1 6 -27 44.40 36.50 -1 6 -27 25.30 28.80 1 -7 -27 12.90 27.60 1 7 -27 -31.50 32.20 1 7 -27 -9.80 20.50 0 -7 -27 -4.70 30.50 0 7 -27 -33.60 22.10 0 7 -27 65.79 35.30 -1 -7 -27 48.80 32.60 -1 7 -27 3.90 37.20 -1 7 -27 23.50 30.50 1 -8 -27 67.39 28.70 1 8 -27 7.50 25.30 1 8 -27 29.00 35.50 0 -8 -27 57.79 29.80 0 8 -27 131.89 35.60 0 8 -27 55.79 29.30 -1 -8 -27 50.39 37.50 -1 8 -27 34.70 29.70 -1 8 -27 42.90 39.40 1 -9 -27 26.20 26.60 1 9 -27 4.30 37.50 1 9 -27 24.70 24.80 0 -9 -27 -21.00 31.00 0 9 -27 -8.30 37.30 0 9 -27 5.10 26.60 0 -10 -27 71.49 34.00 0 10 -27 33.50 42.50 0 10 -27 24.20 30.60 1 0 -28 17.90 30.40 0 0 -28 61.69 29.30 -1 0 -28 -21.70 37.80 1 -1 -28 -0.50 28.40 1 1 -28 57.79 27.40 1 1 -28 66.79 31.60 0 -1 -28 69.89 27.30 0 1 -28 -16.40 25.50 -1 -1 -28 -30.20 33.50 -1 1 -28 22.00 33.30 1 -2 -28 121.79 31.80 1 2 -28 95.49 26.50 1 2 -28 89.09 31.20 0 -2 -28 -16.10 29.90 0 2 -28 -2.10 33.50 -1 -2 -28 33.00 37.80 -1 2 -28 0.70 33.70 1 -3 -28 5.90 25.60 1 3 -28 -11.90 28.60 1 3 -28 -11.80 20.20 0 -3 -28 296.97 47.90 0 3 -28 231.58 48.00 -1 -3 -28 -20.30 33.80 -1 3 -28 30.20 32.50 1 -4 -28 12.00 29.20 1 4 -28 40.60 32.90 1 4 -28 39.40 23.00 0 -4 -28 41.60 32.30 0 4 -28 6.20 22.80 0 4 -28 78.69 36.70 -1 -4 -28 35.10 35.00 -1 4 -28 16.30 38.80 1 -5 -28 25.00 24.90 1 5 -28 1.10 32.50 1 5 -28 -12.90 24.30 0 -5 -28 88.29 33.80 0 5 -28 23.00 37.00 0 5 -28 -44.30 22.70 -1 -5 -28 57.69 41.10 -1 5 -28 -2.60 36.10 1 -6 -28 -0.90 25.60 1 6 -28 8.80 24.70 1 6 -28 -26.50 30.60 0 -6 -28 69.89 35.40 0 6 -28 134.79 40.40 0 6 -28 58.29 27.90 -1 -6 -28 19.20 39.00 -1 6 -28 6.30 44.60 -1 6 -28 -16.20 31.40 1 -7 -28 44.10 26.40 1 7 -28 47.80 36.20 1 7 -28 46.70 26.60 0 -7 -28 56.49 35.10 0 7 -28 25.40 27.80 0 7 -28 89.99 38.80 0 -8 -28 10.00 33.00 0 8 -28 6.60 26.10 0 8 -28 0.00 35.00 1 0 -29 22.30 28.10 0 0 -29 -1.80 29.70 -1 0 -29 -13.40 42.70 1 -1 -29 -3.60 26.70 1 1 -29 6.00 27.70 0 -1 -29 -7.10 29.20 0 1 -29 31.30 30.50 -1 -1 -29 -0.70 36.10 -1 1 -29 -11.00 35.30 1 -2 -29 -6.40 26.60 1 2 -29 34.30 33.70 0 -2 -29 52.39 29.80 0 2 -29 3.20 31.40 -1 -2 -29 -21.40 40.10 -1 2 -29 17.50 37.20 1 -3 -29 71.59 35.00 1 3 -29 139.59 34.20 1 3 -29 110.69 27.20 0 -3 -29 10.30 29.30 0 3 -29 8.50 36.10 1 -4 -29 -24.80 27.10 1 4 -29 57.29 31.80 1 4 -29 -24.80 25.00 0 -4 -29 -16.70 34.40 0 4 -29 27.00 34.60 0 -5 -29 3.70 35.80 0 5 -29 77.49 39.20 0 5 -29 47.80 27.10 0 -6 -29 32.50 36.60 0 6 -29 54.99 41.10 0 0 -30 31.00 39.20 0 -1 -30 27.20 33.00 0 1 -30 -11.80 39.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 71656 _olex2_submission_special_instructions 'No special instructions were received' 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 S1 S 0.9102(4) 0.39752(8) 0.54036(6) 0.0490(5) Uani 1 1 d . . . . . Cl1 Cl 0.9322(5) 0.21680(8) 0.38637(6) 0.0598(6) Uani 1 1 d . . . . . Cl2 Cl 0.8981(6) 0.06634(9) 0.43235(7) 0.0793(7) Uani 1 1 d . . . . . N1 N 0.6466(12) 0.4302(2) 0.39161(16) 0.0408(12) Uani 1 1 d . . . . . N3 N 0.6708(12) 0.3245(2) 0.45582(16) 0.0433(13) Uani 1 1 d . . . . . H3 H 0.601353 0.326440 0.423033 0.052 Uiso 1 1 calc R U . . . N2 N 0.7427(13) 0.4397(2) 0.44439(17) 0.0463(14) Uani 1 1 d . . . . . H2 H 0.788430 0.480298 0.455988 0.056 Uiso 1 1 calc R U . . . C8 C 0.2957(14) 0.5435(3) 0.2300(2) 0.0336(14) Uani 1 1 d . . . . . C13 C 0.3937(14) 0.5424(3) 0.2847(2) 0.0331(14) Uani 1 1 d . . . . . C1 C 0.6490(13) 0.4280(3) 0.2717(2) 0.0312(13) Uani 1 1 d . . . . . C14 C 0.5672(14) 0.4835(3) 0.3057(2) 0.0331(14) Uani 1 1 d . . . . . C7 C 0.3715(15) 0.4872(3) 0.1980(2) 0.0408(15) Uani 1 1 d . . . . . H7 H 0.300231 0.487854 0.162300 0.049 Uiso 1 1 calc R U . . . C6 C 0.5494(14) 0.4299(3) 0.2171(2) 0.0367(14) Uani 1 1 d . . . . . C17 C 0.6709(15) 0.2581(3) 0.4793(2) 0.0375(14) Uani 1 1 d . . . . . C12 C 0.3071(15) 0.5998(3) 0.3161(2) 0.0428(15) Uani 1 1 d . . . . . H12 H 0.364952 0.599900 0.352282 0.051 Uiso 1 1 calc R U . . . C2 C 0.8500(15) 0.3696(3) 0.2886(2) 0.0405(15) Uani 1 1 d . . . . . H2A H 0.927220 0.367133 0.323984 0.049 Uiso 1 1 calc R U . . . C5 C 0.6311(16) 0.3744(3) 0.1832(2) 0.0467(17) Uani 1 1 d . . . . . H5 H 0.555241 0.375185 0.147708 0.056 Uiso 1 1 calc R U . . . C9 C 0.1188(15) 0.6018(3) 0.2092(3) 0.0489(16) Uani 1 1 d . . . . . H9 H 0.051617 0.602680 0.173326 0.059 Uiso 1 1 calc R U . . . C15 C 0.6565(14) 0.4839(3) 0.3622(2) 0.0403(15) Uani 1 1 d . . . . . H15 H 0.724248 0.525119 0.377877 0.048 Uiso 1 1 calc R U . . . C16 C 0.7655(14) 0.3854(3) 0.4781(2) 0.0362(14) Uani 1 1 d . . . . . C4 C 0.8184(16) 0.3199(3) 0.2013(3) 0.0490(17) Uani 1 1 d . . . . . H4 H 0.871783 0.284206 0.178428 0.059 Uiso 1 1 calc R U . . . C10 C 0.0472(16) 0.6558(3) 0.2408(3) 0.0543(18) Uani 1 1 d . . . . . H10 H -0.065481 0.693812 0.226499 0.065 Uiso 1 1 calc R U . . . C18 C 0.5519(16) 0.2457(3) 0.5301(2) 0.0501(17) Uani 1 1 d . . . . . H18 H 0.474244 0.281963 0.550434 0.060 Uiso 1 1 calc R U . . . C22 C 0.7859(15) 0.2020(3) 0.4489(2) 0.0407(15) Uani 1 1 d . . . . . C3 C 0.9293(16) 0.3186(3) 0.2549(2) 0.0495(17) Uani 1 1 d . . . . . H3A H 1.059587 0.281937 0.267448 0.059 Uiso 1 1 calc R U . . . C11 C 0.1409(16) 0.6548(3) 0.2945(3) 0.0555(18) Uani 1 1 d . . . . . H11 H 0.089904 0.692139 0.315973 0.067 Uiso 1 1 calc R U . . . C21 C 0.7720(16) 0.1362(3) 0.4699(2) 0.0474(16) Uani 1 1 d . . . . . C20 C 0.6568(17) 0.1249(3) 0.5200(2) 0.0565(18) Uani 1 1 d . . . . . H20 H 0.651072 0.080555 0.533769 0.068 Uiso 1 1 calc R U . . . C19 C 0.5486(17) 0.1799(3) 0.5503(2) 0.0579(19) Uani 1 1 d . . . . . H19 H 0.473145 0.172200 0.584516 0.070 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0664(12) 0.0496(10) 0.0305(8) -0.0035(7) -0.0091(8) -0.0051(9) Cl1 0.0820(14) 0.0643(11) 0.0338(9) -0.0063(8) 0.0129(8) -0.0042(10) Cl2 0.1088(18) 0.0521(11) 0.0771(13) -0.0124(10) 0.0055(12) 0.0196(11) N1 0.055(4) 0.046(3) 0.020(2) -0.003(2) -0.006(2) -0.008(3) N3 0.067(4) 0.037(3) 0.026(3) 0.001(2) -0.007(2) -0.007(3) N2 0.075(4) 0.036(3) 0.027(3) -0.001(2) -0.012(2) -0.005(3) C8 0.030(3) 0.037(3) 0.034(3) 0.006(3) 0.000(3) -0.008(3) C13 0.039(4) 0.033(3) 0.028(3) 0.003(3) 0.004(3) -0.005(3) C1 0.029(3) 0.029(3) 0.035(3) 0.007(3) 0.005(3) -0.007(3) C14 0.036(4) 0.038(3) 0.025(3) 0.003(3) 0.000(2) -0.010(3) C7 0.046(4) 0.048(4) 0.029(3) 0.004(3) -0.001(3) -0.009(3) C6 0.038(4) 0.037(3) 0.035(3) 0.001(3) 0.008(3) -0.013(3) C17 0.042(4) 0.040(4) 0.031(3) 0.000(3) 0.001(3) -0.009(3) C12 0.045(4) 0.044(4) 0.040(3) -0.001(3) 0.000(3) 0.000(3) C2 0.045(4) 0.042(4) 0.035(3) 0.003(3) 0.008(3) -0.001(3) C5 0.047(4) 0.062(5) 0.032(3) -0.016(3) 0.015(3) -0.015(4) C9 0.041(4) 0.057(4) 0.048(4) 0.012(4) -0.007(3) -0.004(3) C15 0.050(4) 0.036(3) 0.034(3) 0.003(3) -0.005(3) 0.000(3) C16 0.037(4) 0.044(4) 0.028(3) -0.008(3) 0.004(3) -0.003(3) C4 0.050(4) 0.033(4) 0.065(5) -0.015(3) 0.025(3) -0.007(3) C10 0.053(5) 0.042(4) 0.067(5) 0.017(4) -0.004(4) -0.003(3) C18 0.056(5) 0.059(4) 0.036(3) -0.003(3) 0.013(3) -0.002(3) C22 0.044(4) 0.047(4) 0.031(3) -0.004(3) 0.001(3) 0.001(3) C3 0.056(5) 0.045(4) 0.048(4) 0.003(3) 0.017(3) 0.000(3) C11 0.052(5) 0.042(4) 0.073(5) 0.004(4) 0.007(4) 0.003(3) C21 0.057(5) 0.040(4) 0.045(4) -0.009(3) -0.002(3) 0.004(3) C20 0.072(5) 0.048(4) 0.050(4) 0.007(3) 0.002(4) -0.003(4) C19 0.073(5) 0.057(5) 0.044(4) 0.012(4) 0.012(3) -0.013(4) 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' S S 0.1246 0.1234 '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 C15 N1 N2 115.6(5) . . ? C17 N3 H3 115.6 . . ? C16 N3 H3 115.6 . . ? C16 N3 C17 128.8(5) . . ? N1 N2 H2 119.8 . . ? C16 N2 N1 120.5(4) . . ? C16 N2 H2 119.8 . . ? C13 C8 C9 119.1(5) . . ? C7 C8 C13 119.2(5) . . ? C7 C8 C9 121.7(5) . . ? C8 C13 C14 119.0(5) . . ? C8 C13 C12 117.6(5) . . ? C12 C13 C14 123.4(5) . . ? C14 C1 C2 123.8(5) . . ? C6 C1 C14 119.9(5) . . ? C6 C1 C2 116.2(5) . . ? C13 C14 C15 117.2(5) . . ? C1 C14 C13 120.4(5) . . ? C1 C14 C15 122.4(5) . . ? C8 C7 H7 118.5 . . ? C6 C7 C8 122.9(5) . . ? C6 C7 H7 118.5 . . ? C1 C6 C5 119.9(6) . . ? C7 C6 C1 118.5(5) . . ? C7 C6 C5 121.5(5) . . ? C18 C17 N3 122.8(5) . . ? C18 C17 C22 118.8(5) . . ? C22 C17 N3 118.3(5) . . ? C13 C12 H12 119.2 . . ? C11 C12 C13 121.5(6) . . ? C11 C12 H12 119.2 . . ? C1 C2 H2A 118.9 . . ? C3 C2 C1 122.2(5) . . ? C3 C2 H2A 118.9 . . ? C6 C5 H5 119.2 . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.2 . . ? C8 C9 H9 119.6 . . ? C10 C9 C8 120.9(6) . . ? C10 C9 H9 119.6 . . ? N1 C15 C14 123.3(5) . . ? N1 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N3 C16 S1 126.4(4) . . ? N2 C16 S1 119.4(4) . . ? N2 C16 N3 114.2(5) . . ? C5 C4 H4 120.5 . . ? C5 C4 C3 119.0(5) . . ? C3 C4 H4 120.5 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.3(6) . . ? C11 C10 H10 119.9 . . ? C17 C18 H18 119.8 . . ? C19 C18 C17 120.4(6) . . ? C19 C18 H18 119.8 . . ? C17 C22 Cl1 119.2(4) . . ? C21 C22 Cl1 121.4(4) . . ? C21 C22 C17 119.3(5) . . ? C2 C3 C4 121.1(6) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C12 C11 C10 120.6(6) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C22 C21 Cl2 120.1(5) . . ? C20 C21 Cl2 118.9(5) . . ? C20 C21 C22 121.1(6) . . ? C21 C20 H20 120.1 . . ? C21 C20 C19 119.8(6) . . ? C19 C20 H20 120.1 . . ? C18 C19 C20 120.6(6) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? 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 S1 C16 1.664(5) . ? Cl1 C22 1.714(6) . ? Cl2 C21 1.737(6) . ? N1 N2 1.379(6) . ? N1 C15 1.279(6) . ? N3 H3 0.8600 . ? N3 C17 1.420(7) . ? N3 C16 1.358(6) . ? N2 H2 0.8600 . ? N2 C16 1.354(7) . ? C8 C13 1.414(7) . ? C8 C7 1.398(7) . ? C8 C9 1.424(8) . ? C13 C14 1.429(7) . ? C13 C12 1.415(7) . ? C1 C14 1.421(7) . ? C1 C6 1.413(7) . ? C1 C2 1.444(7) . ? C14 C15 1.451(7) . ? C7 H7 0.9300 . ? C7 C6 1.397(8) . ? C6 C5 1.419(8) . ? C17 C18 1.393(7) . ? C17 C22 1.415(8) . ? C12 H12 0.9300 . ? C12 C11 1.361(8) . ? C2 H2A 0.9300 . ? C2 C3 1.347(7) . ? C5 H5 0.9300 . ? C5 C4 1.364(8) . ? C9 H9 0.9300 . ? C9 C10 1.354(8) . ? C15 H15 0.9300 . ? C4 H4 0.9300 . ? C4 C3 1.403(8) . ? C10 H10 0.9300 . ? C10 C11 1.385(8) . ? C18 H18 0.9300 . ? C18 C19 1.377(8) . ? C22 C21 1.387(8) . ? C3 H3A 0.9300 . ? C11 H11 0.9300 . ? C21 C20 1.369(8) . ? C20 H20 0.9300 . ? C20 C19 1.387(8) . ? C19 H19 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 Cl1 C22 C21 Cl2 -1.0(8) . . . . ? Cl1 C22 C21 C20 179.6(5) . . . . ? Cl2 C21 C20 C19 -178.7(5) . . . . ? N1 N2 C16 S1 175.4(4) . . . . ? N1 N2 C16 N3 -3.2(8) . . . . ? N3 C17 C18 C19 178.0(5) . . . . ? N3 C17 C22 Cl1 2.1(7) . . . . ? N3 C17 C22 C21 -176.7(5) . . . . ? N2 N1 C15 C14 179.4(5) . . . . ? C8 C13 C14 C1 1.9(8) . . . . ? C8 C13 C14 C15 -178.6(5) . . . . ? C8 C13 C12 C11 -1.2(8) . . . . ? C8 C7 C6 C1 1.9(8) . . . . ? C8 C7 C6 C5 -178.1(5) . . . . ? C8 C9 C10 C11 -1.0(9) . . . . ? C13 C8 C7 C6 -1.8(8) . . . . ? C13 C8 C9 C10 0.6(9) . . . . ? C13 C14 C15 N1 142.9(6) . . . . ? C13 C12 C11 C10 0.9(9) . . . . ? C1 C14 C15 N1 -37.7(8) . . . . ? C1 C6 C5 C4 -3.0(8) . . . . ? C1 C2 C3 C4 -0.1(9) . . . . ? C14 C13 C12 C11 -179.8(6) . . . . ? C14 C1 C6 C7 0.0(8) . . . . ? C14 C1 C6 C5 180.0(5) . . . . ? C14 C1 C2 C3 -178.4(5) . . . . ? C7 C8 C13 C14 -0.1(8) . . . . ? C7 C8 C13 C12 -178.8(5) . . . . ? C7 C8 C9 C10 179.9(6) . . . . ? C7 C6 C5 C4 176.9(6) . . . . ? C6 C1 C14 C13 -1.9(8) . . . . ? C6 C1 C14 C15 178.7(5) . . . . ? C6 C1 C2 C3 -2.2(8) . . . . ? C6 C5 C4 C3 0.7(9) . . . . ? C17 N3 C16 S1 0.1(9) . . . . ? C17 N3 C16 N2 178.5(5) . . . . ? C17 C18 C19 C20 -1.4(10) . . . . ? C17 C22 C21 Cl2 177.7(5) . . . . ? C17 C22 C21 C20 -1.6(10) . . . . ? C12 C13 C14 C1 -179.4(5) . . . . ? C12 C13 C14 C15 0.0(8) . . . . ? C2 C1 C14 C13 174.1(5) . . . . ? C2 C1 C14 C15 -5.2(8) . . . . ? C2 C1 C6 C7 -176.3(5) . . . . ? C2 C1 C6 C5 3.6(8) . . . . ? C5 C4 C3 C2 0.9(9) . . . . ? C9 C8 C13 C14 179.2(5) . . . . ? C9 C8 C13 C12 0.5(8) . . . . ? C9 C8 C7 C6 178.9(5) . . . . ? C9 C10 C11 C12 0.2(10) . . . . ? C15 N1 N2 C16 -175.1(5) . . . . ? C16 N3 C17 C18 44.6(9) . . . . ? C16 N3 C17 C22 -137.7(6) . . . . ? C18 C17 C22 Cl1 179.9(5) . . . . ? C18 C17 C22 C21 1.1(9) . . . . ? C22 C17 C18 C19 0.4(9) . . . . ? C22 C21 C20 C19 0.7(10) . . . . ? C21 C20 C19 C18 0.8(10) . . . . ?