#------------------------------------------------------------------------------ #$Date: 2025-02-06 01:10:06 +0200 (Thu, 06 Feb 2025) $ #$Revision: 297603 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573849.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_1573849 loop_ _publ_author_name 'Lu, Jiachen' 'Ok, Kang Min' _publ_section_title ; Synergistic engineering of ultraviolet metal-free crystals with exceptional birefringence via pyridine-derived dimers ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D5SC00112A _journal_year 2025 _chemical_formula_moiety 'C5 H4 N O3 S, C5 H7 N2' _chemical_formula_sum 'C10 H11 N3 O3 S' _chemical_formula_weight 253.28 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2024-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-10-25 deposited with the CCDC. 2025-02-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.2257(4) _cell_length_b 13.4248(8) _cell_length_c 24.3820(14) _cell_measurement_reflns_used 7231 _cell_measurement_temperature 303.00 _cell_measurement_theta_max 27.29 _cell_measurement_theta_min 3.03 _cell_volume 2365.1(2) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 303.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 0.0786 _diffrn_reflns_av_unetI/netI 0.0460 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 27477 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.383 _diffrn_reflns_theta_min 3.035 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.274 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6341 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0906 before and 0.0829 after correction. The Ratio of minimum to maximum transmission is 0.8503. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.423 _exptl_crystal_description plate _exptl_crystal_F_000 1056 _refine_diff_density_max 0.231 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 198 _refine_ls_number_reflns 2963 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.209 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0779 _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^)+(0.0250P)^2^+3.0444P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1284 _refine_ls_wR_factor_ref 0.1474 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1994 _reflns_number_total 2963 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d5sc00112a2.cif _cod_data_source_block x _cod_database_code 1573849 _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. ; _olex2_refinement_description ; ; _shelx_res_file ; TITL x_a.res in Pbcn x.res created by SHELXL-2018/3 at 10:54:52 on 14-Oct-2024 REM Old TITL x in Pbcn REM SHELXT solution in Pbcn: R1 0.170, Rweak 0.021, Alpha 0.035 REM 0.923 for 368 systematic absences, Orientation as input REM Formula found by SHELXT: C10 N3 O3 S CELL 0.71073 7.2257 13.4248 24.382 90 90 90 ZERR 8 0.0004 0.0008 0.0014 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S UNIT 80 88 24 24 8 L.S. 4 PLAN 5 TEMP 29.85 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.025000 3.044400 FVAR 0.38287 S001 5 0.876450 0.543545 0.603301 11.00000 0.06322 0.04067 = 0.03072 0.00051 0.00010 -0.00167 O002 4 0.866243 0.436001 0.599240 11.00000 0.07489 0.03776 = 0.05266 0.00322 -0.00873 0.00347 O003 4 1.058397 0.581836 0.590272 11.00000 0.06512 0.07848 = 0.05886 0.01199 -0.01274 -0.02287 O004 4 0.803241 0.580478 0.654807 11.00000 0.11928 0.06758 = 0.02808 -0.00512 0.00836 0.01632 N005 3 0.680012 0.638410 0.458467 11.00000 0.06270 0.04969 = 0.03762 0.00451 -0.00316 0.00200 N006 3 0.762723 0.709370 0.180753 11.00000 0.08540 0.05402 = 0.03410 0.00037 0.00003 0.01490 N007 3 0.739224 0.658445 0.345650 11.00000 0.05885 0.07980 = 0.03462 0.00498 -0.00352 0.00818 C008 1 0.725673 0.589778 0.551741 11.00000 0.05266 0.02875 = 0.03634 -0.00195 0.00393 -0.00113 C009 1 0.789905 0.607530 0.499318 11.00000 0.04871 0.04464 = 0.03551 0.00156 0.00327 0.00091 C00A 1 0.753061 0.692391 0.234747 11.00000 0.04425 0.05187 = 0.03677 -0.00139 -0.00168 0.00790 C00B 1 0.767336 0.595554 0.256150 11.00000 0.06460 0.04882 = 0.04435 -0.00490 -0.00140 0.00785 C00C 1 0.539535 0.604131 0.562340 11.00000 0.05982 0.05062 = 0.05222 0.00523 0.01361 0.00635 C00D 1 0.726883 0.770355 0.272087 11.00000 0.06138 0.05385 = 0.04180 -0.00198 -0.00207 0.01301 C00E 1 0.761465 0.581173 0.311051 11.00000 0.06784 0.05868 = 0.05039 0.01074 -0.00714 0.00675 C00F 1 0.501843 0.652499 0.469818 11.00000 0.06184 0.05168 = 0.05784 0.00300 -0.01212 0.00092 C00G 1 0.719955 0.750680 0.326693 11.00000 0.06336 0.06608 = 0.04434 -0.01303 -0.00181 0.01460 C00H 1 0.426151 0.636066 0.520702 11.00000 0.04854 0.05863 = 0.08146 0.00375 0.00449 0.00665 H009 2 0.916737 0.599194 0.490362 11.00000 0.05208 H00A 2 0.782174 0.659342 0.158537 11.00000 0.06152 H00B 2 0.750279 0.770657 0.167926 11.00000 0.06146 H00F 2 0.424759 0.674712 0.439087 11.00000 0.07177 H00C 2 0.500205 0.588622 0.598262 11.00000 0.07638 H00H 2 0.300188 0.646987 0.527955 11.00000 0.07856 H00G 2 0.773021 0.515295 0.329603 11.00000 0.07463 H00I 2 0.702143 0.805332 0.353492 11.00000 0.07472 H007 2 0.736511 0.646948 0.381339 11.00000 0.08089 H00E 2 0.711845 0.837717 0.256659 11.00000 0.07574 H00D 2 0.780654 0.544134 0.234292 11.00000 0.06222 HKLF 4 REM x_a.res in Pbcn REM wR2 = 0.1474, GooF = S = 1.209, Restrained GooF = 1.209 for all data REM R1 = 0.0779 for 1994 Fo > 4sig(Fo) and 0.1243 for all 2963 data REM 198 parameters refined using 0 restraints END WGHT 0.0250 3.0443 REM Highest difference peak 0.231, deepest hole -0.314, 1-sigma level 0.060 Q1 1 1.0000 0.8885 0.2500 10.50000 0.05 0.23 Q2 1 0.5243 0.5638 0.6911 11.00000 0.05 0.23 Q3 1 0.6277 0.5760 0.5493 11.00000 0.05 0.21 Q4 1 1.0089 0.5612 0.5829 11.00000 0.05 0.21 Q5 1 0.6185 0.5417 0.6329 11.00000 0.05 0.21 ; _shelx_res_checksum 40046 _shelx_hkl_file ; 1 0 0 2.80 0.80 1 0 0 3.10 0.90 -1 0 0 3.00 0.80 -2 0 0 9999.00 425.76 3 0 0 0.50 1.40 -3 0 0 0.60 1.40 3 0 0 0.70 1.80 -3 0 0 0.20 1.60 -3 0 0 0.10 1.60 3 0 0 -0.60 1.30 3 0 0 -0.50 1.50 4 0 0 1027.20 48.50 -4 0 0 1009.70 48.40 -4 0 0 1036.70 50.39 4 0 0 1113.69 50.29 4 0 0 1001.20 49.99 4 0 0 1082.59 48.40 -4 0 0 1113.39 50.29 5 0 0 0.90 3.20 5 0 0 1.20 2.80 -5 0 0 -0.40 4.00 5 0 0 -2.50 2.00 6 0 0 230.88 17.00 6 0 0 241.98 17.60 -6 0 0 238.88 17.90 6 0 0 226.58 15.40 7 0 0 1.60 3.70 -8 0 0 46.00 9.70 8 0 0 48.80 8.50 8 0 0 43.30 8.40 9 0 0 -8.60 4.80 -9 0 0 9.00 5.40 9 0 0 -0.90 6.40 -1 -1 0 1212.48 51.29 -1 1 0 1179.08 50.89 -1 1 0 1180.28 50.59 1 -1 0 1097.29 51.09 2 1 0 2.20 1.20 2 -1 0 1.70 1.40 -2 1 0 0.00 1.50 2 -1 0 1.30 1.50 -2 -1 0 1.10 1.40 -2 1 0 2.70 1.40 2 1 0 3.90 1.20 3 1 0 1717.03 76.69 3 1 0 1607.54 74.89 3 1 0 1728.43 74.79 3 -1 0 1717.03 76.69 3 -1 0 1632.24 76.09 -3 1 0 1778.42 76.79 3 -1 0 1892.71 76.99 3 1 0 1657.93 76.89 -3 1 0 1605.04 75.99 -3 1 0 1603.24 76.59 -3 -1 0 1862.21 77.09 3 -1 0 1839.22 76.19 4 1 0 4.00 2.30 -4 1 0 0.60 2.10 4 1 0 -1.40 1.60 4 -1 0 6.00 2.30 -4 -1 0 3.20 2.20 4 1 0 1.60 1.70 4 -1 0 6.00 2.30 4 1 0 -1.30 2.00 4 -1 0 -0.80 2.10 -4 1 0 4.80 2.10 -4 1 0 1.30 1.90 -4 -1 0 -1.40 1.80 -5 1 0 134.79 11.90 5 -1 0 120.29 10.40 -5 1 0 131.09 10.70 5 -1 0 146.49 11.80 5 -1 0 154.68 10.70 5 1 0 158.38 12.10 -5 -1 0 163.18 12.00 5 1 0 133.79 11.70 5 1 0 132.09 9.80 -5 -1 0 135.89 12.00 5 1 0 150.08 9.90 -5 1 0 161.58 12.20 6 1 0 0.10 2.70 6 1 0 5.80 3.60 6 1 0 3.90 2.90 6 -1 0 1.20 3.50 -7 1 0 5.00 4.60 7 -1 0 14.30 4.50 7 1 0 8.20 4.60 7 1 0 5.20 3.30 7 -1 0 5.60 3.90 -7 -1 0 3.40 4.20 8 -1 0 11.00 5.30 -8 -1 0 -3.60 4.20 -8 1 0 1.10 4.70 8 1 0 -1.60 3.80 8 1 0 0.60 4.40 -9 -1 0 0.70 6.20 9 -1 0 -2.00 5.70 9 1 0 0.00 6.70 -9 1 0 -2.90 6.10 0 2 0 622.54 27.60 1 -2 0 2.00 0.70 -1 2 0 0.70 0.70 1 -2 0 1.10 0.60 -1 -2 0 1.30 0.80 1 2 0 -0.20 0.80 -1 -2 0 1.10 0.80 -1 2 0 1.80 0.80 1 -2 0 1.40 1.10 -1 2 0 0.70 1.10 2 -2 0 1020.00 45.40 2 -2 0 1067.99 46.30 2 -2 0 1040.80 45.50 2 2 0 988.10 45.90 -2 2 0 1073.99 46.50 -2 -2 0 928.41 45.70 -2 2 0 1062.39 45.90 -2 -2 0 997.30 45.80 2 2 0 1000.30 46.10 -3 -2 0 1.00 1.70 3 2 0 3.50 2.10 3 2 0 2.40 1.90 -3 -2 0 3.00 1.90 4 2 0 1212.48 55.29 4 -2 0 1160.68 57.19 4 2 0 1293.87 54.89 4 -2 0 1238.28 57.69 -4 -2 0 1239.68 59.99 4 2 0 1159.08 57.99 4 -2 0 1279.67 57.59 4 2 0 1303.77 58.19 -4 2 0 1333.67 58.19 4 -2 0 1294.07 57.79 -4 -2 0 1072.29 64.19 5 -2 0 1.40 2.50 -5 2 0 -3.00 2.30 5 2 0 3.70 2.20 5 2 0 -0.70 2.30 5 -2 0 3.80 2.70 5 2 0 1.40 1.90 -5 -2 0 5.00 2.80 -5 2 0 1.90 2.50 -6 2 0 15.10 5.80 6 2 0 10.30 4.10 -6 -2 0 18.40 5.10 -6 2 0 8.70 4.50 6 2 0 9.00 3.50 6 -2 0 10.30 4.40 6 -2 0 12.80 4.60 6 2 0 13.10 3.30 7 -2 0 3.20 4.20 7 2 0 11.40 3.90 -7 -2 0 6.00 3.70 7 -2 0 3.90 3.50 8 2 0 3.90 5.20 -8 -2 0 7.90 4.50 8 -2 0 6.40 3.90 8 2 0 2.40 3.90 8 -2 0 6.20 5.50 -8 2 0 2.30 4.70 -9 2 0 -1.70 6.40 9 2 0 12.50 7.10 0 -3 0 0.30 0.90 0 3 0 0.30 1.10 1 3 0 3073.49 129.69 -1 -3 0 3109.89 129.29 1 3 0 2975.20 129.59 -1 3 0 2932.61 128.99 1 -3 0 2997.40 130.79 -1 -3 0 3100.89 129.29 -1 3 0 3055.99 130.89 2 -3 0 -0.60 1.00 -2 3 0 -1.10 1.40 -2 3 0 -0.40 1.10 2 -3 0 0.00 1.00 -2 -3 0 0.60 1.30 -2 3 0 -0.30 1.10 -2 -3 0 -0.10 1.00 2 -3 0 -1.00 1.60 2 3 0 -1.30 1.40 3 -3 0 94.19 7.10 -3 3 0 82.39 7.70 -3 3 0 93.79 7.40 3 3 0 113.39 9.40 -3 3 0 97.89 7.70 3 3 0 100.79 8.00 -3 -3 0 108.19 7.90 3 -3 0 89.89 7.80 3 -3 0 107.29 9.00 -3 -3 0 114.29 8.00 4 3 0 2.20 2.40 -4 -3 0 3.10 2.60 -4 -3 0 -1.60 2.00 -4 3 0 2.20 3.30 -4 3 0 -0.40 1.90 4 -3 0 3.60 2.70 4 -3 0 2.40 2.50 -4 3 0 2.20 2.00 4 3 0 -1.90 2.10 4 -3 0 0.50 2.10 5 3 0 38.50 6.70 -5 3 0 23.10 5.90 5 -3 0 31.60 5.60 -5 -3 0 33.50 5.90 -5 3 0 41.50 6.50 5 3 0 37.20 6.30 5 -3 0 26.90 5.80 -5 3 0 37.90 5.80 -6 3 0 2.50 3.80 6 3 0 -3.90 4.70 6 -3 0 6.70 3.60 -6 3 0 4.30 3.60 -6 -3 0 0.50 2.90 -6 3 0 11.60 4.40 6 3 0 -0.80 3.20 7 -3 0 10.70 5.00 -7 3 0 27.70 7.00 7 -3 0 13.00 4.90 -7 -3 0 21.60 5.70 7 3 0 14.20 5.30 -8 3 0 7.40 4.70 8 3 0 12.80 5.00 8 -3 0 8.70 4.50 -8 -3 0 0.00 4.50 9 3 0 -1.50 6.10 9 -3 0 -7.40 5.10 0 -4 0 3926.81 168.08 1 -4 0 2.50 1.60 1 4 0 1.80 1.00 1 4 0 0.50 1.00 1 4 0 -0.30 1.00 -2 4 0 32.90 4.50 2 -4 0 29.40 2.80 2 4 0 30.60 3.80 -2 -4 0 38.00 3.60 -2 4 0 33.50 3.50 2 -4 0 33.70 4.50 -2 4 0 33.70 3.30 2 -4 0 36.60 3.00 -2 -4 0 37.70 3.60 3 -4 0 1.80 1.50 -3 -4 0 0.80 1.60 -3 4 0 2.60 2.10 -3 -4 0 0.50 1.70 3 -4 0 -2.30 2.00 3 4 0 0.40 1.60 3 4 0 0.20 1.70 -3 4 0 3.60 1.80 3 -4 0 -0.30 1.30 -4 4 0 243.28 16.30 4 -4 0 302.17 16.30 4 4 0 271.27 17.30 4 -4 0 262.37 17.30 -4 -4 0 301.17 17.20 -5 -4 0 1.60 2.40 -5 4 0 -0.20 2.60 5 4 0 -4.30 3.00 -5 4 0 2.60 2.90 5 -4 0 -1.90 2.50 5 4 0 2.80 2.60 -5 4 0 1.70 2.40 6 -4 0 6.30 3.40 -6 -4 0 2.30 3.20 -6 4 0 3.40 3.40 6 -4 0 0.90 3.10 -6 4 0 8.60 3.70 -6 4 0 -4.10 4.10 -7 4 0 9.20 4.30 7 -4 0 8.00 4.10 7 -4 0 -0.90 3.10 7 4 0 2.30 3.80 -7 -4 0 3.50 4.50 -8 4 0 13.70 6.10 8 -4 0 12.20 8.40 8 -4 0 10.80 5.30 -8 -4 0 15.10 5.50 8 4 0 21.50 7.30 9 4 0 4.40 6.60 -9 4 0 8.20 6.10 9 -4 0 4.20 5.80 0 -5 0 -0.10 1.40 0 5 0 0.10 1.40 -1 5 0 7.60 2.30 1 -5 0 7.70 2.20 -2 -5 0 0.00 1.10 2 5 0 -2.40 1.20 -2 5 0 -1.00 1.60 -2 5 0 -0.10 1.10 -2 5 0 -0.70 1.20 2 5 0 0.80 1.50 3 5 0 16.80 3.60 3 -5 0 19.50 3.00 -3 5 0 20.10 4.50 -3 5 0 21.60 3.80 -3 5 0 23.60 3.70 -3 -5 0 25.20 3.70 -3 -5 0 18.20 4.60 4 5 0 -2.60 2.20 4 5 0 2.00 2.50 -4 -5 0 1.70 2.00 4 -5 0 5.50 2.20 -5 -5 0 4.70 2.80 5 -5 0 4.50 3.40 -5 5 0 9.60 3.30 -5 5 0 -0.60 2.90 5 5 0 7.90 4.20 5 5 0 5.80 3.80 5 -5 0 3.40 3.30 -5 5 0 9.90 4.00 -6 5 0 8.10 3.80 -6 5 0 13.30 4.80 -6 5 0 7.00 3.60 -6 -5 0 1.50 3.10 7 -5 0 9.10 4.00 -7 5 0 4.20 4.10 -7 5 0 6.30 4.60 -7 5 0 15.00 6.90 7 5 0 5.60 4.00 -8 -5 0 8.80 5.40 8 5 0 3.40 5.40 9 -5 0 0.80 5.60 -9 5 0 -11.30 6.00 0 -6 0 2884.61 121.39 0 6 0 2681.63 121.09 -1 -6 0 3.00 1.60 1 6 0 6.10 1.90 1 6 0 3.40 1.60 1 6 0 3.00 1.20 -1 6 0 0.80 1.80 1 -6 0 1.40 1.90 -2 -6 0 423.06 19.50 -2 6 0 390.56 20.40 2 6 0 391.66 20.70 2 6 0 403.06 20.80 2 -6 0 442.36 22.80 -2 6 0 426.16 20.00 -2 6 0 396.66 22.80 -3 -6 0 -1.00 1.50 -3 6 0 1.70 1.90 3 6 0 1.00 1.90 -3 6 0 1.30 1.80 -3 6 0 1.40 2.40 4 6 0 15.90 4.20 -4 6 0 24.90 5.30 4 6 0 18.10 4.50 4 -6 0 12.30 3.20 4 -6 0 17.00 4.90 -4 6 0 19.40 4.40 -4 6 0 19.10 4.20 -4 -6 0 23.60 4.20 -5 6 0 4.30 3.30 -5 -6 0 1.10 2.70 5 6 0 3.70 3.20 -5 6 0 2.80 3.20 -5 6 0 -0.70 2.70 5 -6 0 3.00 3.20 -6 -6 0 18.40 4.60 6 -6 0 17.20 5.30 -6 6 0 10.00 4.60 6 -6 0 17.90 4.50 -6 6 0 17.30 6.40 6 6 0 13.60 5.20 -6 6 0 15.50 5.30 6 6 0 18.00 6.00 -7 6 0 5.90 3.80 -7 6 0 5.20 4.00 -7 6 0 1.00 7.40 7 -6 0 4.70 4.30 7 -6 0 4.90 4.00 8 -6 0 -3.70 4.30 8 6 0 1.90 5.40 -9 6 0 8.70 6.80 9 -6 0 5.60 6.80 0 7 0 -0.80 1.60 1 7 0 1305.97 62.89 -1 -7 0 1400.16 62.99 1 -7 0 1549.64 65.39 -1 7 0 1399.66 65.19 -2 7 0 3.40 3.00 -2 7 0 4.70 1.80 -3 7 0 263.67 15.40 3 7 0 290.17 16.90 -3 7 0 233.58 17.40 -3 -7 0 274.77 14.70 -3 7 0 257.57 15.10 3 7 0 292.57 16.60 4 7 0 6.80 3.20 -4 7 0 0.00 2.20 4 -7 0 -3.30 2.70 -4 -7 0 -3.20 2.00 4 7 0 6.60 3.10 -4 7 0 -4.30 2.60 -4 7 0 3.50 3.20 -5 7 0 0.50 3.20 5 -7 0 7.80 3.20 5 7 0 4.00 3.40 -5 -7 0 5.80 3.10 -5 7 0 1.10 3.50 5 7 0 13.60 4.30 6 7 0 4.90 3.70 6 -7 0 3.60 3.60 -6 7 0 11.80 5.80 -6 -7 0 -2.10 3.20 -7 7 0 10.00 8.40 -7 -7 0 5.00 4.70 -7 7 0 1.50 4.60 7 -7 0 10.60 6.30 7 -7 0 3.70 4.30 7 7 0 -1.50 4.70 -7 7 0 2.50 4.10 8 -7 0 -4.30 4.80 0 -8 0 431.86 23.50 0 8 0 355.96 21.10 1 8 0 -0.30 1.90 -1 -8 0 1.50 2.00 -2 8 0 32.10 7.10 2 8 0 29.80 5.10 -2 -8 0 34.00 3.80 2 8 0 35.80 4.00 2 8 0 31.70 4.60 -3 8 0 1.80 1.90 -3 8 0 1.70 2.90 3 8 0 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18.80 6.00 4 -10 21 -1.70 7.00 -4 10 21 -10.20 7.50 4 10 -21 13.60 6.40 -4 10 -21 2.00 5.00 4 10 21 3.80 6.40 5 -10 21 -0.50 8.60 -5 10 21 10.90 7.50 -5 10 21 -2.70 6.90 5 10 -21 7.30 5.70 -5 10 -21 4.10 4.70 5 10 21 1.00 7.90 0 11 21 4.90 5.20 0 11 21 8.30 5.70 0 -11 21 18.30 5.90 0 11 -21 5.30 6.50 1 -11 21 20.10 6.70 -1 11 21 12.80 6.20 -1 11 21 12.10 6.10 1 11 -21 -7.30 6.50 -1 11 -21 5.90 3.50 -1 11 -21 13.10 6.70 -1 -11 21 13.20 6.00 1 11 21 -5.30 5.20 2 11 -21 10.40 5.10 2 -11 21 13.10 7.30 -2 11 21 26.90 8.10 -2 11 21 9.80 6.20 2 11 21 12.50 6.50 -2 11 -21 -2.00 8.20 2 11 21 11.60 6.30 -3 11 21 7.60 6.90 -3 11 21 5.90 6.30 3 11 -21 2.30 4.50 3 -11 21 -4.20 7.20 3 11 21 -5.80 6.20 -3 -11 21 3.70 5.70 -3 11 -21 2.10 4.60 3 11 21 6.30 7.00 -4 11 21 13.90 7.30 4 11 -21 6.10 5.60 4 -11 21 11.00 8.70 -4 11 21 -7.70 6.90 4 11 21 20.20 7.30 -4 11 -21 3.80 4.50 0 12 21 -10.90 5.40 0 -12 21 -11.30 5.80 0 12 -21 -6.30 7.20 0 12 -21 -2.90 3.50 0 12 21 7.60 6.90 1 -12 21 9.70 6.20 1 12 -21 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73.79 10.00 3 0 22 80.39 11.00 -3 0 22 71.69 10.90 -3 0 -22 79.89 10.10 4 0 -22 6.50 5.30 4 0 22 9.60 5.00 -4 0 22 14.20 6.00 -4 0 -22 8.50 5.30 -5 0 22 29.00 7.00 -5 0 22 27.40 7.60 5 0 22 19.50 7.50 -5 0 -22 18.70 6.30 5 0 22 13.20 6.60 5 0 -22 36.80 8.20 6 0 -22 7.20 5.60 -6 0 22 1.60 6.90 -6 0 22 -2.90 5.30 6 0 22 3.10 6.20 -6 0 -22 2.40 5.20 7 0 22 -8.90 7.40 -7 0 -22 5.60 5.90 7 0 -22 0.30 6.30 -7 0 22 2.90 6.10 0 1 -22 -3.30 3.70 0 -1 -22 1.80 3.20 0 1 -22 1.50 2.90 0 -1 22 -0.20 4.00 0 1 22 4.20 4.10 0 -1 22 0.60 3.70 0 1 22 -5.20 3.30 1 1 -22 10.20 4.80 -1 1 22 8.60 4.70 -1 1 22 -1.00 5.10 1 1 -22 4.40 4.20 1 -1 22 8.60 4.70 1 -1 22 13.50 5.70 1 1 22 15.50 5.10 -1 1 -22 9.50 4.20 -1 1 -22 3.00 5.10 1 1 22 14.60 5.40 -1 -1 22 19.50 5.90 -1 -1 22 9.00 4.30 1 -1 -22 11.60 4.50 2 -1 22 150.98 14.70 -2 1 22 194.78 16.20 2 -1 22 178.38 16.70 -2 -1 -22 179.88 15.30 2 1 -22 165.28 15.10 -2 1 22 183.18 16.00 -2 1 -22 158.18 15.00 -2 -1 22 169.48 16.20 2 -1 -22 172.68 17.70 2 1 22 199.78 17.20 2 1 22 146.39 14.90 -2 1 -22 182.48 15.40 -2 -1 22 201.18 16.30 3 -1 22 33.20 7.90 3 1 -22 23.40 6.00 3 -1 22 19.40 6.10 -3 1 22 19.70 6.20 -3 1 22 25.10 7.40 -3 -1 -22 31.10 7.40 -3 1 -22 18.20 6.30 -3 -1 22 29.30 7.70 -3 1 -22 30.50 9.00 3 1 22 24.00 6.80 3 -1 -22 28.80 7.80 -3 -1 22 23.60 6.40 4 -1 22 -1.20 5.20 4 1 -22 0.10 3.90 4 -1 22 -3.50 4.70 -4 1 22 -0.60 4.60 4 1 22 1.60 4.40 -4 1 -22 -6.40 3.30 4 1 22 -6.90 4.80 -4 -1 22 3.90 4.70 -4 -1 22 -5.20 5.10 4 -1 -22 3.50 4.20 5 -1 22 10.90 6.20 5 -1 22 10.00 5.30 5 1 -22 5.60 4.30 -5 -1 -22 4.60 5.00 -5 1 22 8.20 4.60 -5 1 22 -1.40 6.00 -5 1 -22 6.50 3.90 -5 -1 22 -0.40 4.60 5 -1 -22 2.50 4.50 5 1 22 10.80 6.10 5 1 22 9.50 5.20 -5 -1 22 6.10 5.80 -6 -1 -22 58.29 9.90 -6 1 22 54.59 10.40 6 1 -22 36.00 9.20 6 -1 22 55.39 10.80 -6 -1 22 39.30 8.80 -6 -1 22 34.70 11.20 -6 1 -22 54.49 10.60 6 -1 -22 48.40 10.00 6 1 22 29.70 9.60 -7 1 22 -6.20 6.00 7 -1 22 -9.40 7.70 -7 -1 -22 20.60 11.40 7 -1 -22 3.90 8.30 -7 -1 22 -2.80 6.00 -7 1 -22 1.60 5.70 7 1 22 -12.60 7.10 0 -2 22 52.79 8.30 0 2 22 41.60 8.40 0 2 22 43.30 9.00 0 2 -22 34.60 7.60 0 -2 -22 32.50 7.40 0 2 -22 48.20 7.70 -1 2 22 67.39 9.90 -1 2 22 72.89 9.70 -1 -2 -22 54.49 8.50 1 -2 22 44.50 7.90 1 2 -22 55.79 8.70 1 2 -22 72.39 8.90 1 2 22 54.49 9.10 -1 -2 22 58.19 10.40 1 2 22 58.49 9.50 -1 -2 22 52.59 9.00 -1 2 -22 61.99 9.00 1 -2 -22 59.79 9.00 -2 -2 -22 45.30 8.70 -2 2 22 42.20 9.10 2 -2 22 31.80 7.40 2 -2 22 62.29 9.90 2 2 -22 41.60 7.70 2 2 -22 38.80 7.80 -2 2 22 55.79 8.90 2 2 22 54.29 9.50 -2 2 -22 47.50 7.80 2 2 22 40.20 8.40 -2 -2 22 49.60 9.20 -2 2 -22 59.39 8.10 2 -2 -22 50.69 9.50 -2 -2 22 45.10 8.10 -3 -2 -22 86.29 11.20 -3 2 22 83.79 12.00 -3 2 22 104.69 12.20 3 2 -22 89.59 11.10 3 2 -22 115.39 17.70 3 -2 -22 90.79 11.30 3 2 22 99.69 12.00 -3 -2 22 88.09 10.90 3 2 22 113.89 12.00 -3 2 -22 99.29 11.40 -3 -2 22 75.99 11.30 -4 -2 -22 10.50 5.10 4 2 -22 8.50 4.50 -4 2 22 9.30 6.20 4 -2 22 10.50 5.80 4 -2 22 14.60 5.60 4 2 22 12.50 5.90 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7.60 6.20 2 -7 28 -4.50 7.50 -2 7 28 16.10 7.80 -2 -7 28 -5.10 7.20 -2 7 -28 4.80 5.90 2 7 28 -7.90 7.20 -3 7 28 -6.70 7.40 -3 7 28 6.50 8.30 3 -7 28 15.30 8.90 3 7 28 13.90 8.90 -3 -7 28 -2.80 6.50 0 8 28 4.20 7.50 0 -8 28 -2.00 6.90 0 8 -28 -7.90 4.80 1 8 -28 7.40 5.70 -1 8 28 -12.80 7.20 1 -8 28 -6.70 8.00 -1 8 28 1.30 7.90 -1 8 -28 -4.00 5.70 1 8 28 10.30 8.20 -1 -8 28 -8.70 7.60 -2 8 28 -3.50 7.70 -2 8 28 2.50 7.80 -2 8 -28 1.90 5.60 2 8 28 -9.20 7.90 -2 -8 28 7.60 7.40 0 -9 28 -5.10 7.50 0 9 28 13.80 7.20 0 9 28 15.40 9.20 0 0 29 5.30 7.80 0 0 -29 4.80 4.90 0 0 29 7.60 6.20 1 0 29 -9.70 6.40 1 0 -29 -0.60 5.00 -1 0 29 -7.10 5.50 -1 0 29 -4.80 6.90 -1 0 -29 -3.00 4.40 2 0 29 3.10 6.10 2 0 -29 6.80 5.40 -2 0 29 -1.20 6.20 -2 0 -29 -0.90 4.60 3 0 -29 -2.30 5.10 -3 0 -29 0.80 6.50 -3 0 29 6.60 6.10 3 0 29 2.90 6.80 4 0 29 14.00 7.90 -4 0 29 20.40 7.40 0 -1 -29 -5.00 4.70 0 1 -29 -4.10 4.40 0 1 29 -3.70 5.70 0 -1 29 -5.30 6.30 0 1 29 -0.40 6.50 1 1 -29 -5.00 4.70 -1 1 29 -5.10 6.50 1 -1 29 -11.20 5.50 -1 -1 -29 -2.60 4.50 1 1 29 -3.50 6.40 1 -1 -29 0.70 5.10 1 1 29 -3.00 7.00 -1 -1 29 3.70 7.40 -1 1 -29 -0.80 5.20 -2 -1 -29 -7.10 5.30 2 1 -29 -8.90 5.20 -2 1 29 7.20 6.10 -2 1 29 3.00 6.90 2 -1 29 -0.20 6.90 -2 -1 29 -2.80 6.10 -2 1 -29 5.60 5.40 2 1 29 -13.00 6.50 2 -1 -29 -3.90 4.80 3 -1 29 9.70 6.80 -3 -1 -29 10.00 5.50 -3 1 29 -3.50 5.90 3 1 29 -3.60 7.40 3 -1 -29 1.80 5.20 -3 1 -29 5.40 5.60 -3 -1 29 -9.40 6.10 -4 -1 -29 -4.30 7.00 4 1 -29 4.00 6.00 -4 1 29 1.10 7.00 4 -1 29 -1.70 7.70 4 -1 -29 -10.00 6.00 -4 1 -29 2.20 5.60 4 1 29 17.10 8.70 0 2 29 12.70 7.20 0 -2 29 20.10 7.30 0 2 -29 26.40 6.80 0 -2 -29 19.70 7.00 1 2 -29 0.50 4.40 1 -2 29 -0.10 6.30 -1 2 -29 -3.00 4.00 1 -2 -29 -7.50 4.70 1 2 29 4.70 6.60 -1 -2 29 0.80 5.90 -2 2 29 5.60 7.20 -2 2 29 20.00 13.00 -2 -2 -29 -1.90 5.00 2 2 -29 4.00 4.70 2 -2 29 -3.90 6.10 -2 2 -29 -5.40 4.60 2 2 29 8.70 6.70 2 2 29 3.50 7.50 -2 -2 29 3.20 6.00 2 -2 -29 8.30 5.20 3 -2 29 37.80 11.20 -3 -2 -29 38.10 8.00 3 2 -29 27.80 8.80 -3 2 29 23.70 9.90 -3 2 29 36.20 10.80 3 2 29 21.10 9.30 3 -2 -29 30.70 8.20 -3 -2 29 33.90 8.90 -3 2 -29 41.00 8.00 4 -2 29 8.30 8.80 -4 2 29 -8.30 7.10 4 2 -29 2.50 6.20 -4 -2 -29 16.30 6.80 4 -2 -29 -7.50 6.40 4 2 29 14.60 8.00 0 3 29 6.20 6.60 0 3 -29 6.60 4.80 -1 -3 -29 3.50 5.60 1 3 -29 -3.30 4.60 1 -3 29 12.80 7.50 -1 3 29 2.80 6.60 -1 3 29 -0.30 6.10 1 3 29 0.70 6.80 -1 -3 29 -1.90 5.50 1 3 29 16.70 7.40 -1 3 -29 1.30 4.50 1 -3 -29 8.70 5.60 -2 3 29 12.90 7.70 2 -3 29 21.20 9.70 -2 -3 -29 18.90 7.40 2 3 -29 20.20 5.90 -2 3 29 30.00 9.20 -2 3 -29 14.50 6.20 2 3 29 22.60 8.40 2 -3 -29 17.20 6.70 2 3 29 20.90 8.40 -2 -3 29 24.10 8.20 -3 3 29 -4.40 7.90 3 -3 29 18.60 13.80 -3 3 29 7.30 6.90 -3 -3 -29 1.30 6.10 3 3 -29 2.50 5.50 3 3 29 -8.00 10.60 -3 3 -29 2.90 5.30 3 -3 -29 -4.40 6.30 3 3 29 0.30 7.50 -3 -3 29 11.80 6.80 -4 -3 -29 -1.10 6.40 -4 3 29 2.90 7.50 4 -3 29 2.20 8.40 4 3 -29 9.20 5.80 -4 3 -29 8.10 5.50 4 3 29 -5.30 7.80 0 -4 29 8.30 7.10 0 4 29 -5.60 6.10 0 4 -29 -2.20 4.60 0 4 29 -0.20 7.10 -1 -4 -29 5.80 6.00 1 -4 29 -3.30 6.90 -1 4 29 7.90 6.80 -1 4 29 6.30 8.30 1 4 -29 -1.00 4.80 1 4 29 9.60 7.00 -1 4 -29 8.90 5.50 -1 -4 29 10.10 6.60 1 4 29 6.00 8.20 -2 4 29 -8.20 6.80 2 -4 29 6.70 7.60 2 4 -29 0.20 4.80 -2 4 29 3.10 6.90 -2 -4 29 1.10 6.20 2 -4 -29 -5.60 6.00 2 4 29 9.50 7.40 -2 4 -29 -2.30 5.10 2 4 29 -0.30 7.60 3 4 -29 15.40 6.90 -3 -4 -29 6.10 7.40 -3 4 29 15.20 8.50 -3 4 29 17.60 8.70 -3 -4 29 16.90 8.10 -3 4 -29 4.30 5.90 3 4 29 15.10 9.00 3 4 29 15.30 9.50 0 5 29 0.70 7.10 0 -5 -29 2.20 6.40 0 -5 29 -5.80 6.90 0 5 -29 -4.10 4.90 1 5 -29 5.90 4.80 -1 5 29 -4.90 6.60 -1 -5 -29 2.90 7.10 1 -5 29 -8.40 6.70 -1 5 29 10.10 7.40 -1 -5 29 3.70 6.00 1 -5 -29 0.60 7.90 1 5 29 1.10 7.00 1 5 29 1.70 6.80 2 -5 29 36.20 10.50 2 5 -29 37.80 8.90 -2 5 29 33.00 10.00 -2 5 29 22.20 9.70 2 5 29 46.10 10.10 -2 -5 29 36.90 9.90 2 5 29 39.00 10.50 -2 5 -29 27.60 8.00 3 -5 29 21.90 9.30 -3 5 29 17.30 8.20 3 5 -29 16.50 6.10 -3 5 -29 17.70 5.70 -3 -5 29 25.30 7.90 0 6 29 -4.60 6.90 0 -6 29 -7.90 6.20 0 6 29 4.40 7.60 -1 6 29 4.80 7.70 -1 6 29 14.00 9.20 1 6 -29 7.80 5.90 1 -6 29 9.90 7.30 1 6 29 7.90 8.40 -1 6 -29 16.20 6.00 1 6 29 14.20 7.60 -2 6 29 10.00 7.40 -2 6 29 -1.30 8.30 2 6 -29 3.30 5.20 -2 -6 29 -2.00 6.70 2 6 29 -9.80 7.00 0 7 -29 -3.40 5.00 0 7 29 7.20 7.60 0 7 29 4.80 8.20 0 -7 29 1.20 7.20 1 7 -29 -8.90 5.30 1 -7 29 -4.60 7.10 -1 7 29 10.70 6.90 -1 7 29 8.10 7.70 -1 7 -29 2.00 5.30 -1 -7 29 8.70 7.80 1 7 29 -11.10 8.30 1 7 29 12.00 9.20 2 7 -29 29.80 9.10 -2 7 29 28.80 9.80 2 -7 29 35.40 11.00 -2 -7 29 31.00 9.10 2 7 29 33.20 10.20 2 7 29 24.40 9.80 0 8 29 -0.40 7.60 0 8 29 5.30 8.80 0 8 -29 9.30 6.10 0 -8 29 3.30 8.30 0 0 -30 24.70 7.20 0 0 30 31.50 10.30 -1 0 -30 4.40 5.20 -1 0 30 12.70 6.10 1 0 30 18.30 7.30 1 0 -30 5.80 5.40 -2 0 30 -5.20 7.40 2 0 -30 0.80 6.30 -2 0 -30 -11.70 9.50 -3 0 -30 -8.00 6.20 -3 0 30 13.50 6.80 3 0 -30 3.60 8.60 3 0 30 -1.10 8.40 0 -1 30 1.10 7.10 0 -1 -30 -2.50 4.90 0 1 30 -5.90 6.00 -1 -1 -30 20.90 5.80 1 1 -30 11.50 6.50 -1 1 30 8.40 7.20 1 -1 30 28.50 8.20 -1 1 -30 22.40 6.70 1 -1 -30 9.00 6.20 -1 -1 30 17.60 8.30 1 1 30 34.70 9.30 2 -1 30 17.80 8.90 -2 -1 -30 19.60 6.60 -2 1 30 11.60 9.20 -2 -1 30 18.30 8.40 -2 1 -30 15.10 6.70 2 -1 -30 24.30 7.30 2 1 30 13.90 8.90 3 -1 30 23.60 11.40 3 1 -30 12.30 7.20 -3 -1 30 27.70 8.40 -3 1 -30 33.10 8.10 3 1 30 35.90 11.70 3 -1 -30 20.80 8.40 0 2 30 15.20 7.90 0 -2 30 23.10 8.20 0 2 -30 8.80 6.20 0 2 30 2.40 8.00 -1 2 30 -0.10 6.90 1 2 -30 -7.60 4.80 -1 2 30 -0.50 7.40 1 -2 30 -2.30 6.80 -1 -2 -30 7.40 5.80 -1 2 -30 -6.50 4.70 1 -2 -30 -0.80 5.20 1 2 30 2.70 6.90 1 2 30 -6.00 7.00 -1 -2 30 -8.70 6.30 2 2 -30 6.00 5.90 -2 -2 -30 11.80 5.60 -2 2 30 6.20 6.90 2 2 30 5.00 7.10 -2 2 -30 9.00 5.30 -2 -2 30 17.30 7.30 3 -2 30 23.00 9.50 3 2 -30 11.40 6.50 -3 -2 -30 14.40 6.80 -3 2 30 20.00 8.40 3 -2 -30 12.90 7.40 -3 2 -30 2.40 6.80 -3 -2 30 30.50 8.50 3 2 30 10.40 9.60 0 -3 -30 7.50 5.50 0 3 30 4.70 6.80 0 -3 30 7.60 7.30 0 3 -30 4.10 4.70 1 -3 30 14.70 8.10 1 3 -30 7.70 6.10 -1 3 30 17.30 8.00 -1 -3 -30 19.70 7.00 1 3 30 17.60 8.30 -1 -3 30 18.10 7.70 1 -3 -30 16.30 6.60 1 3 30 7.30 7.90 -1 3 -30 19.50 6.10 -2 3 30 -1.70 7.80 -2 3 30 14.90 7.70 -2 -3 -30 1.90 6.20 2 3 -30 0.10 5.20 2 3 30 -11.10 11.70 -2 3 -30 -4.80 6.00 -2 -3 30 9.90 7.20 2 3 30 11.00 13.10 -3 3 30 9.40 14.20 3 3 -30 6.00 5.70 -3 -3 -30 9.60 6.80 3 -3 30 3.10 7.80 3 3 30 10.00 8.00 3 -3 -30 3.50 11.70 -3 3 -30 17.90 6.50 0 -4 -30 0.80 6.90 0 4 30 22.10 7.70 0 4 -30 12.90 6.20 0 4 30 9.50 8.00 -1 -4 -30 6.50 6.90 1 4 -30 10.70 5.90 -1 4 30 5.60 7.10 1 -4 30 5.50 7.60 -1 4 30 13.60 8.60 1 -4 -30 3.00 6.40 1 4 30 1.30 8.00 -1 4 -30 7.20 5.90 -1 -4 30 0.10 7.10 1 4 30 14.70 9.00 -2 -4 -30 8.30 7.00 2 4 -30 -1.50 5.60 -2 4 30 -10.50 13.00 -2 4 30 -4.70 8.10 2 4 30 3.90 7.90 -2 -4 30 4.30 7.50 -2 4 -30 -0.50 5.90 -3 4 30 14.00 8.80 -3 4 30 6.70 8.40 3 4 -30 9.30 6.00 3 -4 30 0.80 8.10 -3 4 -30 -7.80 5.40 3 4 30 -9.40 7.20 0 5 30 7.90 7.40 0 5 -30 4.30 4.90 0 -5 30 22.00 8.50 1 -5 30 12.20 8.10 -1 5 30 15.60 8.10 -1 -5 30 -9.50 6.90 1 5 30 6.70 7.20 -1 5 -30 2.10 5.50 2 -5 30 7.00 7.90 -2 5 30 -3.10 7.20 -2 5 30 -7.00 7.40 2 5 -30 -9.00 5.10 -2 5 -30 -0.30 5.60 2 5 30 -6.70 7.30 2 5 30 -16.70 8.40 0 6 30 2.20 7.80 0 6 30 -11.90 8.40 0 -6 30 -0.70 7.90 0 6 -30 -10.40 5.20 -1 6 30 -13.10 8.70 -1 6 30 3.40 7.70 1 6 -30 2.30 5.60 1 -6 30 12.40 11.30 -1 6 -30 3.10 5.60 1 6 30 2.10 8.80 1 6 30 19.20 8.30 0 0 31 11.10 7.10 -1 0 31 0.50 6.80 1 0 31 7.00 8.10 -1 0 -31 17.60 5.70 -2 0 31 2.90 7.50 2 0 -31 14.40 11.40 0 1 31 0.80 6.50 0 -1 31 7.30 6.80 0 -1 -31 -2.00 5.60 1 1 -31 -2.40 5.60 1 -1 31 -7.80 7.40 -1 -1 -31 -7.70 5.50 1 -1 -31 1.60 5.70 -1 -1 31 7.40 8.20 -1 1 -31 10.00 5.90 1 1 31 -12.10 8.40 -2 1 31 10.50 8.20 2 1 -31 -3.60 6.30 2 1 31 0.00 8.00 -2 -1 31 -15.00 7.00 2 -1 -31 4.40 5.60 -2 1 -31 10.30 6.20 0 -2 31 -8.70 6.50 0 2 31 4.70 8.20 0 2 -31 0.00 4.90 -1 2 31 2.50 7.20 1 -2 31 21.50 8.00 1 -2 -31 5.10 6.10 -1 2 -31 6.30 5.00 -2 -2 -31 4.30 6.20 -2 2 31 10.70 9.80 2 -2 31 2.60 7.70 2 2 -31 0.00 5.60 2 -2 -31 8.70 6.30 2 2 31 -6.80 6.70 -2 2 -31 0.50 5.80 0 3 31 14.50 10.60 0 3 -31 1.70 5.20 0 -3 31 4.40 7.20 0 -3 -31 -8.20 6.00 -1 3 31 1.10 11.30 -1 -3 -31 -2.10 6.50 1 3 -31 1.10 5.70 1 -3 31 9.30 9.20 -1 -3 31 -6.40 7.40 1 3 31 16.90 8.10 1 -3 -31 3.80 6.60 -1 3 -31 6.80 5.50 -2 3 31 5.90 8.20 2 -3 31 14.40 8.40 -2 -3 -31 -3.00 6.60 2 -3 -31 9.70 6.60 -2 -3 31 10.80 7.80 -2 3 -31 15.70 5.90 2 3 31 8.30 7.90 0 4 31 1.00 8.10 0 -4 -31 10.50 9.20 0 4 -31 12.80 5.80 0 4 31 11.30 8.60 0 -4 31 -9.40 8.00 1 4 -31 4.60 5.90 -1 4 31 11.70 8.40 -1 -4 -31 3.50 11.50 -1 -4 31 12.20 7.70 1 4 31 4.50 7.50 -1 4 -31 8.00 5.60 1 4 31 -2.00 8.70 0 5 31 -11.80 7.80 0 -5 31 13.50 9.30 0 5 31 4.20 7.60 0 5 -31 5.10 5.70 -1 5 31 12.40 8.10 1 -5 31 20.50 10.20 1 5 -31 3.50 5.80 -1 5 -31 9.10 6.20 -1 -5 31 10.50 8.10 1 5 31 8.40 8.00 0 0 -32 11.60 6.00 0 0 32 10.40 8.40 -1 0 -32 5.20 6.20 1 0 32 4.20 8.30 1 0 -32 -2.30 5.90 0 1 32 -3.00 7.30 0 1 -32 7.20 5.80 0 -1 32 0.40 12.20 -1 -1 -32 -2.90 7.30 -1 1 32 13.30 8.60 1 -1 32 3.50 7.40 1 1 32 19.40 8.30 1 -1 -32 -7.20 7.30 -1 1 -32 -5.90 6.00 0 2 32 7.00 7.90 0 -2 32 9.60 9.80 0 -2 -32 5.20 6.30 0 2 -32 12.80 6.30 1 -2 32 35.10 11.90 -1 2 32 18.40 9.20 -1 -2 -32 9.00 8.00 -1 2 -32 23.90 7.80 1 2 32 31.70 10.60 0 3 32 6.50 7.90 0 -3 -32 4.40 7.10 0 -3 32 7.60 8.90 0 3 -32 5.80 6.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 53007 _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+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, 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 S001 S 0.87645(13) 0.54355(6) 0.60330(3) 0.0449(2) Uani 1 1 d . . . . . O002 O 0.8662(4) 0.43600(16) 0.59924(10) 0.0551(7) Uani 1 1 d . . . . . O003 O 1.0584(4) 0.5818(2) 0.59027(10) 0.0675(8) Uani 1 1 d . . . . . O004 O 0.8032(5) 0.5805(2) 0.65481(9) 0.0716(9) Uani 1 1 d . . . . . N005 N 0.6800(4) 0.6384(2) 0.45847(11) 0.0500(7) Uani 1 1 d . . . . . N006 N 0.7627(5) 0.7094(3) 0.18075(12) 0.0578(9) Uani 1 1 d . . . . . N007 N 0.7392(5) 0.6584(3) 0.34565(13) 0.0578(9) Uani 1 1 d . . . . . C008 C 0.7257(5) 0.5898(2) 0.55174(12) 0.0393(7) Uani 1 1 d . . . . . C009 C 0.7899(5) 0.6075(3) 0.49932(13) 0.0430(8) Uani 1 1 d . . . . . C00A C 0.7531(5) 0.6924(3) 0.23475(12) 0.0443(8) Uani 1 1 d . . . . . C00B C 0.7673(6) 0.5956(3) 0.25615(15) 0.0526(9) Uani 1 1 d . . . . . C00C C 0.5395(6) 0.6041(3) 0.56234(16) 0.0542(10) Uani 1 1 d . . . . . C00D C 0.7269(6) 0.7704(3) 0.27209(14) 0.0523(9) Uani 1 1 d . . . . . C00E C 0.7615(6) 0.5812(3) 0.31105(16) 0.0590(10) Uani 1 1 d . . . . . C00F C 0.5018(6) 0.6525(3) 0.46982(17) 0.0571(10) Uani 1 1 d . . . . . C00G C 0.7200(6) 0.7507(3) 0.32669(15) 0.0579(10) Uani 1 1 d . . . . . C00H C 0.4262(6) 0.6361(3) 0.52070(19) 0.0629(11) Uani 1 1 d . . . . . H009 H 0.917(5) 0.599(3) 0.4904(13) 0.052(10) Uiso 1 1 d . . . . . H00A H 0.782(5) 0.659(3) 0.1585(15) 0.062(12) Uiso 1 1 d . . . . . H00B H 0.750(5) 0.771(3) 0.1679(15) 0.061(12) Uiso 1 1 d . . . . . H00F H 0.425(6) 0.675(3) 0.4391(15) 0.072(12) Uiso 1 1 d . . . . . H00C H 0.500(6) 0.589(3) 0.5983(16) 0.076(13) Uiso 1 1 d . . . . . H00H H 0.300(6) 0.647(3) 0.5280(16) 0.079(13) Uiso 1 1 d . . . . . H00G H 0.773(6) 0.515(3) 0.3296(16) 0.075(12) Uiso 1 1 d . . . . . H00I H 0.702(5) 0.805(3) 0.3535(16) 0.075(13) Uiso 1 1 d . . . . . H007 H 0.737(6) 0.647(3) 0.3813(17) 0.081(14) Uiso 1 1 d . . . . . H00E H 0.712(6) 0.838(3) 0.2567(16) 0.076(13) Uiso 1 1 d . . . . . H00D H 0.781(5) 0.544(3) 0.2343(14) 0.062(12) Uiso 1 1 d . . . . . 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 S001 0.0632(6) 0.0407(4) 0.0307(4) 0.0005(3) 0.0001(4) -0.0017(4) O002 0.0749(18) 0.0378(13) 0.0527(14) 0.0032(10) -0.0087(13) 0.0035(12) O003 0.0651(18) 0.078(2) 0.0589(16) 0.0120(14) -0.0127(14) -0.0229(15) O004 0.119(3) 0.0676(18) 0.0281(12) -0.0051(11) 0.0084(14) 0.0163(17) N005 0.063(2) 0.0497(18) 0.0376(15) 0.0045(13) -0.0032(13) 0.0020(15) N006 0.085(3) 0.054(2) 0.0341(15) 0.0004(16) 0.0000(16) 0.0149(19) N007 0.059(2) 0.080(3) 0.0346(16) 0.0050(16) -0.0035(15) 0.0082(18) C008 0.053(2) 0.0287(16) 0.0363(16) -0.0019(13) 0.0039(15) -0.0011(15) C009 0.049(2) 0.045(2) 0.0355(16) 0.0016(14) 0.0033(15) 0.0009(17) C00A 0.0443(19) 0.052(2) 0.0368(16) -0.0014(15) -0.0017(15) 0.0079(16) C00B 0.065(3) 0.049(2) 0.0444(19) -0.0049(17) -0.0014(18) 0.0078(19) C00C 0.060(2) 0.051(2) 0.052(2) 0.0052(18) 0.0136(19) 0.0064(19) C00D 0.061(2) 0.054(2) 0.0418(18) -0.0020(17) -0.0021(18) 0.0130(19) C00E 0.068(3) 0.059(2) 0.050(2) 0.0107(19) -0.007(2) 0.007(2) C00F 0.062(3) 0.052(2) 0.058(2) 0.0030(19) -0.012(2) 0.001(2) C00G 0.063(3) 0.066(3) 0.044(2) -0.013(2) -0.0018(18) 0.015(2) C00H 0.049(2) 0.059(3) 0.081(3) 0.004(2) 0.004(2) 0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 O002 S001 O004 112.41(16) . . ? O002 S001 C008 105.59(15) . . ? O003 S001 O002 112.66(17) . . ? O003 S001 O004 113.59(18) . . ? O003 S001 C008 106.13(15) . . ? O004 S001 C008 105.65(16) . . ? C00F N005 C009 117.6(3) . . ? C00A N006 H00A 119(2) . . ? C00A N006 H00B 120(2) . . ? H00A N006 H00B 121(3) . . ? C00E N007 H007 119(3) . . ? C00G N007 C00E 120.8(3) . . ? C00G N007 H007 120(3) . . ? C009 C008 S001 120.6(3) . . ? C009 C008 C00C 118.4(3) . . ? C00C C008 S001 120.9(3) . . ? N005 C009 C008 122.9(3) . . ? N005 C009 H009 116(2) . . ? C008 C009 H009 121(2) . . ? N006 C00A C00B 121.3(3) . . ? N006 C00A C00D 121.3(3) . . ? C00D C00A C00B 117.4(3) . . ? C00A C00B H00D 121(2) . . ? C00E C00B C00A 119.8(4) . . ? C00E C00B H00D 119(2) . . ? C008 C00C H00C 116(3) . . ? C00H C00C C008 119.0(4) . . ? C00H C00C H00C 125(3) . . ? C00A C00D H00E 117(2) . . ? C00G C00D C00A 119.8(4) . . ? C00G C00D H00E 123(2) . . ? N007 C00E C00B 120.9(4) . . ? N007 C00E H00G 114(2) . . ? C00B C00E H00G 125(2) . . ? N005 C00F C00H 123.4(4) . . ? N005 C00F H00F 116(2) . . ? C00H C00F H00F 121(2) . . ? N007 C00G C00D 121.2(4) . . ? N007 C00G H00I 118(2) . . ? C00D C00G H00I 120(2) . . ? C00C C00H C00F 118.7(4) . . ? C00C C00H H00H 119(3) . . ? C00F C00H H00H 122(3) . . ? 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 S001 O002 1.449(2) . ? S001 O003 1.447(3) . ? S001 O004 1.450(2) . ? S001 C008 1.776(3) . ? N005 C009 1.340(4) . ? N005 C00F 1.330(5) . ? N006 C00A 1.338(4) . ? N006 H00A 0.87(4) . ? N006 H00B 0.88(4) . ? N007 C00E 1.347(5) . ? N007 C00G 1.329(5) . ? N007 H007 0.88(4) . ? C008 C009 1.381(4) . ? C008 C00C 1.383(5) . ? C009 H009 0.95(4) . ? C00A C00B 1.405(5) . ? C00A C00D 1.400(5) . ? C00B C00E 1.353(5) . ? C00B H00D 0.88(4) . ? C00C C00H 1.373(6) . ? C00C H00C 0.94(4) . ? C00D C00G 1.358(5) . ? C00D H00E 0.99(4) . ? C00E H00G 1.00(4) . ? C00F C00H 1.374(6) . ? C00F H00F 0.98(4) . ? C00G H00I 0.99(4) . ? C00H H00H 0.94(4) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S001 C008 C009 N005 177.1(3) . . . . ? S001 C008 C00C C00H -177.3(3) . . . . ? O002 S001 C008 C009 -89.2(3) . . . . ? O002 S001 C008 C00C 87.5(3) . . . . ? O003 S001 C008 C009 30.6(3) . . . . ? O003 S001 C008 C00C -152.7(3) . . . . ? O004 S001 C008 C009 151.5(3) . . . . ? O004 S001 C008 C00C -31.8(3) . . . . ? N005 C00F C00H C00C 0.5(6) . . . . ? N006 C00A C00B C00E 178.4(4) . . . . ? N006 C00A C00D C00G -179.2(4) . . . . ? C008 C00C C00H C00F 0.1(6) . . . . ? C009 N005 C00F C00H -0.7(6) . . . . ? C009 C008 C00C C00H -0.5(5) . . . . ? C00A C00B C00E N007 1.0(6) . . . . ? C00A C00D C00G N007 0.6(6) . . . . ? C00B C00A C00D C00G 1.3(6) . . . . ? C00C C008 C009 N005 0.3(5) . . . . ? C00D C00A C00B C00E -2.1(6) . . . . ? C00E N007 C00G C00D -1.7(6) . . . . ? C00F N005 C009 C008 0.3(5) . . . . ? C00G N007 C00E C00B 0.9(6) . . . . ?