#------------------------------------------------------------------------------ #$Date: 2024-10-23 03:36:13 +0300 (Wed, 23 Oct 2024) $ #$Revision: 295586 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/16/01/7160189.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_7160189 loop_ _publ_author_name 'Liu, Lanqin' 'Guo, Shengkun' 'Chen, Chengjun' 'Shen, Xiaoyu' 'Chen, Xiao Yun' 'Yu, Huaguang' 'Han, Ying' 'Sun, Qiu' 'Zhu, Shaoqun' 'Hou, Hong' _publ_section_title ; Visible-light Photoredox-Catalyzed Three-Component Radical Alkyl-Acylation of [1.1.1]Propellane ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D4OB01549E _journal_year 2024 _chemical_formula_moiety 'C17 H22 O S' _chemical_formula_sum 'C17 H22 O S' _chemical_formula_weight 274.40 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc2hpq75 _audit_creation_date 2023-12-16 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6439) ; _audit_update_record ; 2023-12-16 deposited with the CCDC. 2024-10-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.669(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.4888(10) _cell_length_b 17.779(3) _cell_length_c 13.5432(19) _cell_measurement_reflns_used 7089 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 24.535 _cell_measurement_theta_min 2.291 _cell_volume 1530.1(4) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_unetI/netI 0.0384 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 23519 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.512 _diffrn_reflns_theta_min 2.291 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.202 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.6968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1329 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.9347. 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 1.191 _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.263 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 3512 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0587 _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^)+(0.0727P)^2^+0.6262P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1443 _refine_ls_wR_factor_ref 0.1666 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2144 _reflns_number_total 3512 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01549e2.cif _cod_data_source_block gsk123 _cod_database_code 7160189 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.980 _shelx_estimated_absorpt_t_min 0.974 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B) 2.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4) 2.c Idealised Me refined as rotating group: C17(H17A,H17B,H17C) ; _shelx_res_file ; TITL gsk123_a.res in P2(1)/n gsk123.res created by SHELXL-2018/3 at 14:40:43 on 16-Dec-2023 REM Old TITL GSK123 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.232, Rweak 0.032, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C18 S CELL 0.71073 6.4888 17.7786 13.5432 90 101.669 90 ZERR 4 0.001 0.0028 0.0019 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O S UNIT 68 88 4 4 L.S. 10 PLAN 5 0 0 SIZE 0.1 0.12 0.13 TEMP 0 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.072700 0.626200 FVAR 0.93284 S1 4 0.536755 0.328279 0.754256 11.00000 0.05152 0.09548 = 0.06227 0.01054 0.02060 0.00310 O1 3 1.122382 0.364706 0.587799 11.00000 0.03280 0.13499 = 0.06150 0.00798 0.00743 -0.00561 C1 1 0.787696 0.333597 0.818281 11.00000 0.05170 0.07582 = 0.03510 0.00933 0.00704 0.01503 AFIX 43 H1 2 0.829592 0.327975 0.887721 11.00000 -1.20000 AFIX 0 C2 1 0.922142 0.347405 0.753677 11.00000 0.04058 0.07792 = 0.04800 -0.00087 0.00111 0.00345 AFIX 43 H2 2 1.067183 0.351865 0.774776 11.00000 -1.20000 AFIX 0 C3 1 0.816979 0.354093 0.652077 11.00000 0.03716 0.04681 = 0.04266 -0.00316 0.00663 0.00011 C4 1 0.605638 0.345524 0.642522 11.00000 0.04014 0.06753 = 0.04424 0.00084 0.00746 -0.00057 AFIX 43 H4 2 0.509911 0.348779 0.581479 11.00000 -1.20000 AFIX 0 C5 1 0.930783 0.365951 0.569847 11.00000 0.03596 0.05805 = 0.04808 -0.00410 0.00730 -0.00429 C6 1 0.816203 0.379133 0.464137 11.00000 0.03808 0.05476 = 0.04071 -0.00197 0.01072 -0.00193 C7 1 0.928486 0.391233 0.376296 11.00000 0.05026 0.09726 = 0.05470 0.00211 0.01697 -0.00104 AFIX 23 H7A 2 1.002053 0.347939 0.356811 11.00000 -1.20000 H7B 2 1.008138 0.437538 0.377848 11.00000 -1.20000 AFIX 0 C8 1 0.690578 0.396585 0.328417 11.00000 0.04626 0.04839 = 0.03915 -0.00145 0.01362 0.00031 C9 1 0.669164 0.444963 0.421467 11.00000 0.07422 0.06320 = 0.04428 -0.00570 0.01316 0.00803 AFIX 23 H9A 2 0.733513 0.494409 0.425497 11.00000 -1.20000 H9B 2 0.531561 0.445098 0.439134 11.00000 -1.20000 AFIX 0 C10 1 0.662802 0.327204 0.393171 11.00000 0.07070 0.06000 = 0.04233 0.00369 0.00217 -0.01267 AFIX 23 H10A 2 0.524745 0.320928 0.409215 11.00000 -1.20000 H10B 2 0.721594 0.280440 0.374367 11.00000 -1.20000 AFIX 0 C11 1 0.595100 0.411404 0.218817 11.00000 0.05478 0.05423 = 0.03843 0.00357 0.01657 0.00072 C12 1 0.640083 0.344418 0.155830 11.00000 0.08938 0.06188 = 0.04378 -0.00091 0.01928 0.00149 AFIX 23 H12A 2 0.790552 0.341272 0.159096 11.00000 -1.20000 H12B 2 0.596799 0.298642 0.184896 11.00000 -1.20000 AFIX 0 C13 1 0.528224 0.349148 0.045741 11.00000 0.13031 0.07608 = 0.04366 -0.00374 0.02425 -0.00411 AFIX 23 H13A 2 0.584529 0.391046 0.013692 11.00000 -1.20000 H13B 2 0.554097 0.303426 0.011099 11.00000 -1.20000 AFIX 0 C14 1 0.297595 0.359413 0.036665 11.00000 0.11757 0.12279 = 0.04652 0.00898 -0.00350 -0.03331 AFIX 23 H14A 2 0.239041 0.314575 0.061165 11.00000 -1.20000 H14B 2 0.232161 0.365632 -0.033867 11.00000 -1.20000 AFIX 0 C15 1 0.246309 0.426532 0.095098 11.00000 0.06630 0.16007 = 0.05338 0.02636 0.00660 0.01177 AFIX 23 H15A 2 0.095436 0.428960 0.090875 11.00000 -1.20000 H15B 2 0.289204 0.472115 0.065433 11.00000 -1.20000 AFIX 0 C16 1 0.357425 0.421970 0.205394 11.00000 0.06115 0.12126 = 0.04328 0.01182 0.01515 0.01400 AFIX 23 H16A 2 0.299491 0.380255 0.237091 11.00000 -1.20000 H16B 2 0.329836 0.467745 0.239482 11.00000 -1.20000 AFIX 0 C17 1 0.699792 0.482534 0.187473 11.00000 0.09410 0.06360 = 0.06294 0.00975 0.02562 -0.00535 AFIX 137 H17A 2 0.673117 0.524113 0.228347 11.00000 -1.50000 H17B 2 0.642930 0.493381 0.117854 11.00000 -1.50000 H17C 2 0.848788 0.474580 0.196622 11.00000 -1.50000 AFIX 0 HKLF 4 REM gsk123_a.res in P2(1)/n REM wR2 = 0.1666, GooF = S = 1.030, Restrained GooF = 1.030 for all data REM R1 = 0.0587 for 2144 Fo > 4sig(Fo) and 0.1067 for all 3512 data REM 173 parameters refined using 0 restraints END WGHT 0.0723 0.6293 REM Highest difference peak 0.263, deepest hole -0.252, 1-sigma level 0.042 Q1 1 0.8460 0.3345 0.8003 11.00000 0.05 0.26 Q2 1 0.5594 0.3644 0.4137 11.00000 0.05 0.23 Q3 1 0.7074 0.3128 0.7917 11.00000 0.05 0.20 Q4 1 0.5949 0.3421 0.6949 11.00000 0.05 0.19 Q5 1 0.7033 0.3442 0.8019 11.00000 0.05 0.19 ; _shelx_res_checksum 93494 _shelx_hkl_file ; 1 0 0 0.10 0.60 1 0 0 0.60 0.80 -1 0 0 0.60 1.00 -1 0 0 -0.10 0.70 -1 0 0 0.60 0.70 -1 0 0 0.00 0.90 2 0 0 258.67 7.90 -2 0 0 266.67 8.80 -2 0 0 263.97 7.90 -2 0 0 264.07 9.30 -2 0 0 258.77 8.80 3 0 0 -1.00 2.90 3 0 0 -0.90 2.00 -3 0 0 -0.30 2.90 -3 0 0 1.70 2.40 -3 0 0 -2.30 3.20 -3 0 0 0.50 2.60 4 0 0 167.68 8.00 -4 0 0 172.58 8.30 -4 0 0 168.48 9.40 -4 0 0 159.68 9.50 -4 0 0 175.38 10.80 -4 0 0 141.69 9.00 -5 0 0 -3.80 3.50 -5 0 0 0.20 6.10 -5 0 0 10.40 5.90 -5 0 0 2.80 4.90 -5 0 0 -10.30 5.20 -5 0 0 7.30 4.60 -6 0 0 19.20 7.30 -6 0 0 -4.50 4.80 -6 0 0 -13.70 6.20 -6 0 0 -10.00 6.40 -6 0 0 21.30 9.70 -7 0 0 -2.30 6.90 -7 0 0 1.50 9.30 -7 0 0 -4.50 9.50 -8 0 0 48.50 13.60 -8 0 0 56.39 10.30 -8 0 0 38.00 14.00 -8 0 1 4.10 13.60 -8 0 1 7.40 9.30 -8 0 1 -8.10 11.70 -7 0 1 63.39 10.70 -7 0 1 76.59 12.30 -7 0 1 87.59 9.90 -6 0 1 1.80 5.10 -6 0 1 -2.00 8.70 -6 0 1 -3.10 7.30 -6 0 1 -5.50 5.80 -6 0 1 -2.50 7.20 -5 0 1 740.53 24.50 -5 0 1 727.13 21.80 -5 0 1 718.03 23.20 -5 0 1 753.92 24.70 -5 0 1 729.23 24.70 -5 0 1 724.63 21.50 -4 0 1 1.80 4.80 -4 0 1 -7.90 3.30 -4 0 1 1.40 3.40 -4 0 1 1.10 3.60 -4 0 1 -2.30 2.30 -4 0 1 -3.40 3.50 4 0 -1 -2.30 2.90 -3 0 1 216.98 9.10 -3 0 1 205.28 8.70 -3 0 1 205.08 8.20 3 0 -1 197.68 9.80 3 0 -1 205.28 8.40 -2 0 1 -2.00 1.50 -2 0 1 2.40 1.70 -2 0 1 -0.60 1.30 -2 0 1 0.20 1.80 2 0 -1 -0.80 1.30 2 0 -1 0.60 2.00 -1 0 1 4424.76 91.09 -1 0 1 4464.85 91.49 -1 0 1 4356.16 91.99 1 0 -1 4351.06 92.09 1 0 -1 4564.54 91.49 0 0 1 -0.20 0.20 0 0 1 0.00 0.20 0 0 1 -0.30 0.20 0 0 -1 0.40 0.30 0 0 -1 0.30 0.20 0 0 -1 0.00 0.20 1 0 1 3405.06 71.59 1 0 1 3517.65 72.29 1 0 1 3417.16 70.49 -1 0 -1 3409.36 71.39 -1 0 -1 3514.25 72.19 -1 0 -1 3387.86 70.49 2 0 1 1.20 1.90 2 0 1 -1.20 1.20 2 0 1 0.90 2.10 -2 0 -1 1.50 1.40 -2 0 -1 4.10 2.10 -2 0 -1 0.90 1.80 3 0 1 17.70 2.90 3 0 1 17.50 3.90 -3 0 -1 16.00 4.00 -3 0 -1 13.40 2.60 -3 0 -1 15.00 4.10 -3 0 -1 20.90 3.50 4 0 1 2.10 3.90 4 0 1 2.20 2.80 -4 0 -1 2.80 3.50 -4 0 -1 15.80 5.10 -4 0 -1 0.10 3.60 -4 0 -1 -2.20 3.90 -4 0 -1 -5.50 3.00 -5 0 -1 243.08 11.20 -5 0 -1 270.27 14.70 -5 0 -1 249.28 10.50 -5 0 -1 256.37 13.10 -5 0 -1 248.78 14.80 -5 0 -1 255.97 14.60 -6 0 -1 4.50 4.60 -6 0 -1 2.50 6.00 -6 0 -1 6.20 9.80 -6 0 -1 6.60 6.70 -7 0 -1 2.00 9.50 -7 0 -1 13.30 6.40 -7 0 -1 17.80 9.40 -8 0 -1 13.00 12.60 -8 0 -1 0.00 13.40 -8 0 2 -10.90 13.20 -8 0 2 17.80 9.90 -8 0 2 21.90 13.60 -7 0 2 5.60 9.50 -7 0 2 -17.50 9.60 -6 0 2 47.90 6.90 -6 0 2 41.90 8.30 -6 0 2 53.09 10.20 -6 0 2 65.39 10.70 -5 0 2 3.90 5.10 -5 0 2 -7.30 5.60 -5 0 2 -5.40 4.60 -5 0 2 -0.30 4.70 -5 0 2 -4.40 5.80 -5 0 2 5.50 4.40 -4 0 2 242.68 12.10 -4 0 2 243.58 10.70 -4 0 2 241.88 10.50 -4 0 2 246.68 11.00 -4 0 2 241.68 10.10 4 0 -2 224.88 12.50 -3 0 2 1.00 2.40 -3 0 2 -5.20 2.40 -3 0 2 2.90 3.20 -3 0 2 0.10 2.40 3 0 -2 0.80 2.50 3 0 -2 -3.00 3.20 -2 0 2 35.40 2.90 -2 0 2 39.30 3.30 -2 0 2 36.20 3.00 -2 0 2 35.10 3.90 2 0 -2 37.00 3.20 -1 0 2 0.80 1.00 -1 0 2 0.50 0.60 -1 0 2 -0.80 1.00 1 0 -2 0.80 0.60 1 0 -2 -0.10 0.80 1 0 -2 5.50 1.50 0 0 2 3456.95 70.99 0 0 2 3496.05 71.09 0 0 -2 3403.76 71.09 0 0 -2 3437.26 70.89 1 0 2 -0.40 1.10 1 0 2 -1.70 1.10 1 0 2 0.30 0.50 -1 0 -2 -0.40 1.10 -1 0 -2 1.30 0.40 -1 0 -2 0.90 0.80 2 0 2 2300.77 48.70 2 0 2 2258.77 52.19 2 0 2 2329.67 51.09 -2 0 -2 2275.37 48.50 -2 0 -2 2433.46 52.29 -2 0 -2 2296.37 50.29 3 0 2 1.30 2.00 3 0 2 -4.00 2.60 -3 0 -2 3.40 3.00 -3 0 -2 1.20 1.90 -3 0 -2 0.20 2.50 4 0 2 335.57 14.80 4 0 2 313.37 10.80 -4 0 -2 355.06 14.50 -4 0 -2 336.47 14.90 -4 0 -2 318.87 10.70 -4 0 -2 337.37 11.00 -4 0 -2 333.27 12.60 -5 0 -2 -5.70 7.00 -5 0 -2 3.70 3.50 -5 0 -2 3.20 4.10 -5 0 -2 5.00 4.80 -5 0 -2 2.50 6.00 -6 0 -2 71.99 9.00 -6 0 -2 74.59 9.00 -6 0 -2 70.59 7.30 -6 0 -2 71.19 12.10 -6 0 -2 79.79 12.20 -7 0 -2 6.00 6.40 -7 0 -2 -4.10 11.20 -7 0 -2 -7.60 8.40 -8 0 3 20.70 11.70 -8 0 3 12.30 13.80 -7 0 3 52.59 8.30 -7 0 3 46.00 13.80 -6 0 3 2.10 6.50 -6 0 3 7.40 7.90 -6 0 3 -1.60 6.20 -6 0 3 -8.10 8.80 -6 0 3 -9.20 5.40 -5 0 3 91.99 8.10 -5 0 3 94.69 8.30 -5 0 3 99.99 10.50 -5 0 3 98.09 8.80 -5 0 3 74.89 8.50 5 0 -3 95.89 11.50 -4 0 3 4.00 3.80 -4 0 3 1.30 3.20 -4 0 3 2.20 3.10 -4 0 3 1.50 4.70 -4 0 3 0.30 3.20 4 0 -3 5.10 4.30 -3 0 3 1365.96 33.10 -3 0 3 1379.36 32.60 -3 0 3 1394.76 33.60 -3 0 3 1397.06 32.40 -3 0 3 1403.16 34.90 3 0 -3 1333.47 33.20 3 0 -3 1346.97 35.60 -2 0 3 0.70 1.40 -2 0 3 4.00 2.00 -2 0 3 2.60 2.30 2 0 -3 3.40 2.40 2 0 -3 0.40 1.20 2 0 -3 0.40 1.60 -1 0 3 1438.86 31.70 -1 0 3 1418.86 30.10 -1 0 3 1455.65 32.50 -1 0 3 1435.36 31.90 1 0 -3 1397.96 30.20 1 0 -3 1471.95 33.00 0 0 3 1.10 0.80 0 0 3 1.60 0.70 0 0 3 -0.20 0.90 0 0 -3 1.60 0.90 0 0 -3 0.20 0.80 0 0 -3 0.60 0.80 1 0 3 1685.43 35.90 1 0 3 1579.64 33.70 -1 0 -3 1599.04 33.60 -1 0 -3 1685.23 37.00 -1 0 -3 1646.64 35.30 2 0 3 4.70 2.40 2 0 3 1.10 1.00 2 0 3 -1.80 2.00 -2 0 -3 -4.40 2.20 -2 0 -3 0.30 0.90 3 0 3 1472.75 35.30 3 0 3 1402.96 31.40 3 0 3 1396.66 36.70 -3 0 -3 1406.36 33.30 -3 0 -3 1396.46 31.00 -3 0 -3 1409.66 36.00 4 0 3 3.50 4.20 4 0 3 -3.50 5.10 -4 0 -3 -0.80 3.00 -4 0 -3 4.60 2.50 -4 0 -3 -8.40 4.30 -4 0 -3 5.20 2.70 -5 0 -3 41.50 8.70 -5 0 -3 27.20 7.20 -5 0 -3 33.20 5.00 -5 0 -3 25.00 4.10 -5 0 -3 33.10 5.70 -6 0 -3 -26.00 10.60 -6 0 -3 -14.80 5.40 -6 0 -3 -8.60 4.20 -6 0 -3 7.30 9.20 -6 0 -3 -0.50 6.10 -7 0 -3 124.79 13.80 -7 0 -3 105.79 9.90 -7 0 -3 86.69 15.20 -8 0 4 15.70 9.80 -8 0 4 13.00 12.80 -8 0 4 13.50 15.60 -7 0 4 1.40 11.00 -7 0 4 -3.30 6.40 -7 0 4 10.20 8.60 -6 0 4 11.70 5.90 -6 0 4 16.50 9.10 -6 0 4 5.20 7.40 -6 0 4 14.80 5.90 -5 0 4 -1.70 4.20 -5 0 4 6.80 6.10 -5 0 4 -1.70 4.60 -5 0 4 9.70 5.70 -5 0 4 3.50 4.00 5 0 -4 4.60 7.00 -4 0 4 212.88 9.50 -4 0 4 199.98 9.50 -4 0 4 213.38 11.70 -4 0 4 206.88 9.80 -4 0 4 202.38 10.40 4 0 -4 227.68 13.00 -3 0 4 -1.00 2.00 -3 0 4 -0.20 3.30 -3 0 4 3.40 2.80 -3 0 4 -1.00 2.20 3 0 -4 -2.30 3.70 -2 0 4 1807.12 40.60 -2 0 4 1834.42 41.50 -2 0 4 1762.42 37.90 -2 0 4 1702.83 40.00 2 0 -4 1769.82 38.10 2 0 -4 1697.83 41.90 -1 0 4 0.20 1.40 -1 0 4 -0.60 1.50 -1 0 4 0.10 0.70 -1 0 4 -0.30 1.50 1 0 -4 1.70 1.70 1 0 -4 -0.70 0.80 0 0 4 109.19 3.80 0 0 4 115.29 4.50 0 0 4 115.89 4.40 0 0 -4 108.79 3.90 0 0 -4 106.09 4.70 0 0 -4 109.99 4.30 1 0 4 -1.20 0.60 1 0 4 0.20 1.50 1 0 4 -3.30 2.00 -1 0 -4 1.10 0.70 -1 0 -4 1.40 1.90 -1 0 -4 0.10 1.50 2 0 4 1919.71 39.90 2 0 4 1888.81 45.40 2 0 4 1905.61 43.60 -2 0 -4 1893.31 39.40 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7 65.39 5.20 1 3 -7 -0.50 2.30 1 3 -7 1.50 2.60 1 3 -7 0.20 2.40 -1 -3 7 0.70 2.70 -1 -3 7 0.90 2.10 -1 -3 7 2.60 2.80 2 3 -7 125.69 7.30 2 3 -7 131.49 8.70 -2 -3 7 132.19 7.70 -2 -3 7 116.29 6.80 -2 -3 7 126.89 5.90 3 3 -7 33.80 4.80 3 3 -7 43.30 7.10 3 3 -7 33.60 5.10 -3 -3 7 33.60 4.10 -3 -3 7 46.90 6.00 -3 -3 7 35.20 5.80 4 3 -7 124.19 10.90 4 3 -7 117.69 9.10 4 3 -7 133.29 8.70 -4 -3 7 123.19 9.90 -4 -3 7 120.09 9.60 -4 -3 7 135.49 7.90 5 3 -7 37.20 9.80 5 3 -7 26.60 6.80 -5 -3 7 37.20 6.20 -5 -3 7 25.90 6.50 6 3 -7 39.80 11.10 -6 -3 7 53.99 8.40 -6 -3 7 54.99 10.10 -6 -3 7 57.89 9.10 -7 -3 7 14.00 10.00 -7 -3 7 25.40 9.50 -8 -3 7 58.19 13.80 -8 -3 7 31.60 18.70 -8 -3 7 22.90 11.80 -7 3 -6 -27.20 14.90 -7 3 -6 13.60 9.90 -6 3 -6 -8.90 8.20 6 -3 6 -9.70 10.40 -5 3 -6 242.38 13.00 -4 3 -6 -6.80 4.10 4 -3 6 7.70 7.80 4 -3 6 -1.20 6.50 -3 3 -6 450.05 15.00 -3 3 -6 418.96 16.80 3 -3 6 432.96 17.80 3 -3 6 475.55 18.40 -2 3 -6 61.59 5.20 -2 3 -6 69.39 6.40 2 -3 6 62.89 6.90 2 -3 6 60.19 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7.60 -4 -3 5 73.79 7.50 -4 -3 5 91.49 7.10 5 3 -5 514.55 21.80 5 3 -5 491.95 18.90 -5 -3 5 490.55 17.90 -5 -3 5 489.05 18.30 -5 -3 5 484.15 18.30 6 3 -5 305.67 19.40 -6 -3 5 328.17 16.40 -6 -3 5 295.27 17.80 -7 -3 5 13.20 8.10 -8 -3 5 72.19 13.60 -8 -3 5 54.29 17.20 -8 -3 5 64.09 14.80 -7 3 -4 0.20 13.10 -7 3 -4 7.40 9.60 -6 3 -4 8.70 3.60 -6 3 -4 8.50 7.30 6 -3 4 10.70 10.60 -5 3 -4 -1.90 2.60 -5 3 -4 3.00 5.40 -5 3 -4 6.10 3.50 5 -3 4 13.70 9.90 5 -3 4 4.30 7.50 -4 3 -4 185.28 11.70 -4 3 -4 177.98 6.40 -4 3 -4 188.88 5.80 -4 3 -4 176.28 10.20 4 -3 4 188.78 13.30 4 -3 4 199.38 12.30 -3 3 -4 618.04 18.60 -3 3 -4 606.84 13.70 -3 3 -4 633.64 13.40 -3 3 -4 613.94 19.60 3 -3 4 610.84 20.30 3 -3 4 621.44 20.60 -2 3 -4 36.80 4.70 -2 3 -4 33.50 3.70 2 -3 4 42.90 5.00 2 -3 4 44.40 4.80 -1 3 -4 664.83 17.60 -1 3 -4 629.64 16.80 -1 3 -4 654.13 14.20 1 -3 4 645.54 17.70 1 -3 4 639.74 17.60 1 -3 4 654.93 13.90 0 3 -4 22.80 2.60 0 3 -4 22.80 2.30 0 3 -4 26.20 2.60 0 -3 4 24.60 2.90 0 -3 4 26.00 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13.40 -5 11 -5 3.00 8.40 5 -11 5 -4.20 9.70 -4 11 -5 54.99 6.00 -4 11 -5 45.90 8.80 4 -11 5 57.59 6.00 4 -11 5 66.39 13.90 -3 11 -5 47.60 5.60 -3 11 -5 37.10 7.90 3 -11 5 38.00 5.00 3 -11 5 34.80 7.40 -2 11 -5 5.60 3.10 -2 11 -5 1.70 4.30 2 -11 5 2.80 4.60 2 -11 5 7.00 3.00 -1 11 -5 47.30 7.00 -1 11 -5 60.69 6.60 -1 11 -5 44.50 5.20 1 -11 5 44.50 7.70 1 -11 5 46.90 6.60 1 -11 5 38.10 4.40 0 11 -5 -0.50 3.40 0 11 -5 1.30 3.40 0 11 -5 1.90 4.90 0 -11 5 -2.60 3.40 0 -11 5 -0.60 4.60 0 -11 5 0.20 3.00 1 11 -5 61.29 7.70 1 11 -5 59.49 6.30 1 11 -5 50.69 5.40 -1 -11 5 58.99 6.70 -1 -11 5 82.19 7.30 -1 -11 5 52.09 5.80 2 11 -5 8.60 4.00 2 11 -5 10.60 6.50 2 11 -5 9.00 4.70 -2 -11 5 14.30 4.60 -2 -11 5 4.80 4.50 -2 -11 5 7.50 5.20 3 11 -5 12.20 5.70 3 11 -5 18.00 5.10 -3 -11 5 13.70 5.50 -3 -11 5 21.60 4.70 4 11 -5 95.99 10.80 -4 -11 5 86.19 8.10 -4 -11 5 100.29 10.40 5 11 -5 -9.30 7.60 5 11 -5 6.80 8.10 -5 -11 5 5.90 5.30 -5 -11 5 -7.70 6.90 6 11 -5 9.40 10.10 6 11 -5 31.10 11.00 -6 -11 5 23.90 10.00 7 11 -5 -11.00 13.10 -7 -11 5 -4.20 12.80 -6 11 -4 13.60 10.80 6 -11 4 8.10 12.00 -5 11 -4 12.10 4.40 -5 11 -4 18.10 8.80 5 -11 4 -0.70 9.50 -4 11 -4 17.90 8.00 -4 11 -4 21.50 4.20 4 -11 4 16.80 5.00 -3 11 -4 237.48 14.50 -3 11 -4 223.48 8.90 3 -11 4 217.78 13.00 3 -11 4 213.18 9.20 -2 11 -4 16.50 5.00 -2 11 -4 20.70 3.80 -2 11 -4 22.00 7.20 2 -11 4 17.90 5.40 2 -11 4 24.70 3.70 -1 11 -4 2.80 4.50 -1 11 -4 7.60 3.20 -1 11 -4 3.30 3.60 1 -11 4 0.00 2.80 1 -11 4 -2.20 3.70 1 -11 4 -0.90 6.00 0 11 -4 -6.70 4.40 0 11 -4 -2.60 2.80 0 11 -4 3.20 3.20 0 -11 4 -6.70 2.50 0 -11 4 3.70 4.40 0 -11 4 -1.00 3.20 1 11 -4 502.25 16.80 1 11 -4 475.25 15.30 1 11 -4 500.85 18.50 -1 -11 4 492.45 17.20 -1 -11 4 491.45 15.70 -1 -11 4 501.25 17.00 2 11 -4 29.30 4.40 2 11 -4 32.40 5.80 2 11 -4 19.40 6.40 -2 -11 4 31.70 5.00 -2 -11 4 35.40 5.70 -2 -11 4 30.90 5.80 3 11 -4 19.50 4.80 3 11 -4 5.30 5.80 -3 -11 4 13.40 5.40 -3 -11 4 17.50 4.30 4 11 -4 127.89 10.50 -4 -11 4 116.69 11.80 -4 -11 4 112.19 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12 -4 59.09 6.70 0 -12 4 51.99 6.80 0 -12 4 60.19 5.90 0 -12 4 70.49 8.60 1 12 -4 4.50 5.50 1 12 -4 -0.30 3.60 1 12 -4 3.80 3.30 -1 -12 4 6.60 4.10 -1 -12 4 -3.00 3.30 -1 -12 4 -4.00 4.80 2 12 -4 109.49 8.90 2 12 -4 102.69 7.40 2 12 -4 116.99 11.20 -2 -12 4 96.69 8.20 -2 -12 4 128.49 9.50 -2 -12 4 109.39 8.70 3 12 -4 34.30 7.20 3 12 -4 41.90 6.00 -3 -12 4 31.10 7.00 -3 -12 4 35.10 5.70 4 12 -4 76.69 10.10 -4 -12 4 69.89 7.80 -4 -12 4 79.09 12.50 5 12 -4 6.90 7.50 5 12 -4 13.10 8.20 -5 -12 4 13.20 8.60 -5 -12 4 4.40 5.30 6 12 -4 5.20 11.40 -6 -12 4 -9.40 10.10 7 12 -4 9.60 12.50 -7 -12 4 -30.30 14.40 -6 12 -3 10.30 13.10 6 -12 3 27.10 12.60 -5 12 -3 26.30 9.90 -5 12 -3 27.10 5.50 5 -12 3 19.60 10.80 -4 12 -3 90.29 6.60 4 -12 3 110.39 13.80 4 -12 3 87.59 9.70 -3 12 -3 20.20 4.10 3 -12 3 21.00 6.10 3 -12 3 28.90 5.10 -2 12 -3 42.70 5.10 -2 12 -3 34.70 7.60 -2 12 -3 43.50 6.80 2 -12 3 48.20 6.60 2 -12 3 36.60 4.50 -1 12 -3 7.40 3.50 -1 12 -3 13.80 5.30 -1 12 -3 12.40 4.30 1 -12 3 12.20 4.60 1 -12 3 14.80 3.40 1 -12 3 9.80 7.10 0 12 -3 12.60 5.20 0 12 -3 10.10 3.60 0 12 -3 7.50 3.90 0 -12 3 8.10 3.90 0 -12 3 6.70 3.50 0 -12 3 10.60 5.70 1 12 -3 8.00 3.30 1 12 -3 3.00 5.00 1 12 -3 8.00 4.00 -1 -12 3 12.70 5.20 -1 -12 3 11.40 4.70 -1 -12 3 19.00 3.90 2 12 -3 7.10 6.40 2 12 -3 3.80 2.80 2 12 -3 0.60 3.80 -2 -12 3 1.30 4.40 -2 -12 3 16.10 5.10 -2 -12 3 3.40 4.00 3 12 -3 71.59 8.60 3 12 -3 76.79 7.20 -3 -12 3 72.59 7.20 -3 -12 3 78.99 9.60 4 12 -3 97.59 9.10 -4 -12 3 96.09 13.40 -4 -12 3 98.29 7.70 5 12 -3 54.79 9.90 5 12 -3 46.20 9.40 -5 -12 3 49.40 10.40 -5 -12 3 56.69 6.10 6 12 -3 6.70 10.00 -6 -12 3 13.70 12.30 7 12 -3 8.70 14.30 -7 -12 3 -8.20 15.90 -6 12 -2 1.80 11.20 -6 12 -2 -0.30 5.50 6 -12 2 -1.50 10.90 -5 12 -2 0.00 8.90 -5 12 -2 3.90 4.80 5 -12 2 7.00 8.60 5 -12 2 -13.60 7.90 -4 12 -2 13.80 4.20 4 -12 2 5.10 5.30 4 -12 2 16.70 6.50 -3 12 -2 3.90 3.60 -3 12 -2 7.60 5.60 3 -12 2 7.50 5.10 3 -12 2 4.70 4.30 -2 12 -2 72.39 8.60 -2 12 -2 77.99 6.10 -2 12 -2 85.69 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32.10 6.50 -3 12 -1 80.49 10.40 -3 12 -1 61.09 7.90 -3 12 -1 77.99 6.30 3 -12 1 80.79 7.40 3 -12 1 74.89 9.10 -2 12 -1 7.60 4.70 -2 12 -1 17.40 5.40 -2 12 -1 2.60 2.90 2 -12 1 9.00 3.80 2 -12 1 2.30 7.00 2 -12 1 4.80 4.00 -1 12 -1 2.10 2.80 -1 12 -1 -4.40 4.20 -1 12 -1 -0.40 3.60 1 -12 1 4.20 3.50 1 -12 1 -1.50 6.00 1 -12 1 1.80 3.30 0 12 -1 225.98 11.70 0 12 -1 232.68 10.50 0 12 -1 232.08 10.10 0 -12 1 246.18 9.60 0 -12 1 251.47 12.60 0 -12 1 239.18 11.20 1 12 -1 120.19 8.00 1 12 -1 142.59 10.00 1 12 -1 132.69 6.90 -1 -12 1 136.69 9.10 -1 -12 1 125.19 9.20 -1 -12 1 140.79 7.60 2 12 -1 99.89 5.60 2 12 -1 92.39 10.30 2 12 -1 106.39 8.90 -2 -12 1 96.09 7.50 -2 -12 1 104.09 7.60 -2 -12 1 91.29 8.70 3 12 -1 -2.50 4.70 3 12 -1 7.20 3.40 -3 -12 1 7.10 4.20 -3 -12 1 3.40 5.40 4 12 -1 26.40 5.10 4 12 -1 19.40 7.00 -4 -12 1 26.20 4.00 -5 -12 1 27.60 9.40 6 12 -1 12.30 9.50 -6 -12 1 2.10 10.60 7 12 -1 7.70 12.70 -7 -12 1 0.70 14.20 -7 12 0 10.20 16.30 7 -12 0 11.70 15.80 -6 12 0 -15.30 6.20 -6 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-1 49.50 15.00 -3 21 -1 11.80 11.00 3 -21 1 1.10 13.20 -2 21 -1 -26.00 11.40 -2 21 -1 -26.30 8.60 2 -21 1 22.90 10.30 -1 21 -1 5.40 9.90 -1 21 -1 -14.30 9.40 1 -21 1 13.30 9.70 0 21 -1 0.70 8.80 0 -21 1 2.90 9.40 1 21 -1 -8.50 7.10 1 21 -1 11.70 9.70 -1 -21 1 -0.70 11.00 2 21 -1 -3.10 10.60 -2 -21 1 -16.60 10.50 3 21 -1 -19.00 13.30 -3 -21 1 -0.10 11.90 -3 21 0 6.60 13.70 -3 21 0 1.50 10.90 3 -21 0 -16.10 10.50 -2 21 0 9.80 9.00 -2 21 0 -21.40 11.50 2 -21 0 18.00 11.50 -1 21 0 -8.10 8.30 -1 21 0 -1.40 9.30 1 -21 0 -3.40 10.60 0 21 0 -6.30 8.60 0 21 0 1.90 8.80 0 -21 0 -12.70 10.90 1 21 0 -9.60 9.00 1 21 0 9.20 7.10 -1 -21 0 7.30 9.90 2 21 0 15.90 10.50 -2 -21 0 14.30 12.60 3 21 0 4.30 13.60 -3 -21 0 7.70 12.50 -3 21 1 -9.70 8.90 -3 21 1 0.30 13.80 3 -21 -1 14.10 12.40 -2 21 1 4.10 11.70 -2 21 1 -5.20 8.50 2 -21 -1 4.60 11.00 -1 21 1 -6.60 8.10 -1 21 1 -1.70 9.70 1 -21 -1 -2.50 9.80 0 21 1 2.30 8.70 0 21 1 -17.00 9.30 0 -21 -1 -11.20 10.50 1 21 1 -5.80 9.60 1 21 1 -5.60 6.90 -1 -21 -1 9.20 9.90 2 21 1 17.70 12.30 -2 -21 -1 -2.90 10.80 3 21 1 -9.80 12.10 -3 -21 -1 11.00 14.10 -3 21 2 -20.90 13.20 -3 21 2 -5.50 8.70 3 -21 -2 12.70 11.90 -2 21 2 -14.80 11.30 -2 21 2 15.90 9.20 2 -21 -2 -0.90 10.50 -1 21 2 19.70 11.90 -1 21 2 2.40 8.20 1 -21 -2 0.90 10.20 0 21 2 15.60 9.70 0 21 2 8.90 8.60 0 -21 -2 -19.90 9.70 1 21 2 3.20 9.40 -1 -21 -2 -9.60 10.10 2 21 2 23.60 11.00 -2 -21 -2 10.10 11.50 3 21 2 10.10 12.20 -3 -21 -2 8.00 12.40 -3 21 3 -4.60 14.30 -3 21 3 -2.40 9.20 3 -21 -3 -1.00 11.70 -2 21 3 18.90 12.20 -2 21 3 28.60 9.10 2 -21 -3 26.20 11.30 -1 21 3 7.30 9.20 1 -21 -3 2.00 9.30 0 21 3 21.70 9.10 0 21 3 21.90 10.70 0 -21 -3 8.70 9.80 1 21 3 11.00 10.10 -1 -21 -3 8.30 10.80 2 21 3 16.20 11.30 -2 -21 -3 0.50 13.30 -3 21 4 24.30 15.20 -3 21 4 8.60 9.30 3 -21 -4 10.60 11.70 -2 21 4 5.60 8.80 -2 21 4 4.90 12.50 2 -21 -4 16.80 11.30 -1 21 4 2.40 8.60 1 -21 -4 -9.50 9.70 0 21 4 23.30 9.60 0 21 4 8.40 9.50 0 -21 -4 16.00 10.90 1 21 4 -3.70 11.10 -1 -21 -4 -6.10 12.20 2 21 4 -21.90 11.00 -2 -21 -4 11.00 12.40 -2 21 5 8.60 10.40 -2 21 5 -3.00 13.40 2 -21 -5 -7.10 10.80 -1 21 5 11.50 9.30 1 -21 -5 6.60 10.90 0 21 5 -15.50 8.70 0 -21 -5 -16.80 10.80 1 21 5 -8.10 11.40 -1 -21 -5 -15.10 12.90 2 21 5 10.80 12.00 -2 -21 -5 -1.50 12.30 -2 21 6 -4.40 10.30 -2 21 6 7.70 15.20 2 -21 -6 2.70 11.50 -1 21 6 18.60 9.60 1 -21 -6 24.10 11.20 0 21 6 27.00 10.20 0 -21 -6 -0.90 10.90 1 21 6 7.60 10.90 -1 -21 -6 -11.30 13.40 -1 21 7 -1.00 10.80 1 -21 -7 13.50 11.50 0 21 7 23.50 12.00 0 -21 -7 -12.20 12.00 0 22 -5 0.80 11.60 0 22 -5 -15.70 10.70 0 -22 5 -3.80 13.90 1 22 -5 -8.30 12.70 1 22 -5 -4.80 11.30 -1 -22 5 -3.90 12.40 -1 22 -4 -1.30 11.10 -1 22 -4 0.20 12.90 1 -22 4 17.10 12.40 0 22 -4 -2.70 10.70 0 22 -4 2.90 13.30 0 -22 4 -13.10 11.40 1 22 -4 7.50 12.30 1 22 -4 8.50 10.60 -1 -22 4 12.30 11.90 2 22 -4 6.40 13.60 -2 -22 4 -3.90 13.30 -1 22 -3 -10.90 10.40 -1 22 -3 14.40 11.20 1 -22 3 -23.70 10.90 0 22 -3 0.00 9.80 0 22 -3 21.10 11.40 0 -22 3 4.90 12.10 1 22 -3 0.40 9.70 1 22 -3 7.20 12.20 -1 -22 3 -25.80 10.90 2 22 -3 -8.60 12.40 -2 -22 3 -4.90 11.80 -2 22 -2 1.60 10.40 -2 22 -2 -31.40 11.60 2 -22 2 -6.40 12.10 -1 22 -2 0.10 11.50 -1 22 -2 3.60 11.20 1 -22 2 2.40 11.10 0 22 -2 -2.60 10.10 0 22 -2 7.00 12.50 0 -22 2 -25.70 10.40 1 22 -2 10.00 11.80 -1 -22 2 -4.80 12.90 2 22 -2 21.50 12.90 -2 -22 2 1.60 12.80 -2 22 -1 -0.80 10.50 -2 22 -1 3.40 12.40 2 -22 1 -3.40 11.10 -1 22 -1 -11.80 9.90 -1 22 -1 -17.20 10.20 1 -22 1 10.70 10.90 0 22 -1 -9.80 9.80 0 22 -1 -1.70 10.90 0 -22 1 -0.10 10.90 1 22 -1 0.80 11.50 -1 -22 1 -3.90 10.60 2 22 -1 14.70 12.20 -2 -22 1 -14.20 11.80 -2 22 0 3.60 10.20 -2 22 0 -14.70 12.50 2 -22 0 1.90 12.50 -1 22 0 6.00 11.10 -1 22 0 -1.10 10.70 1 -22 0 5.90 10.60 0 22 0 8.70 10.30 0 -22 0 15.30 10.90 1 22 0 19.30 11.30 -1 -22 0 -6.80 10.80 2 22 0 -16.40 12.20 -2 -22 0 12.10 12.20 -2 22 1 5.10 12.40 -2 22 1 7.70 10.40 2 -22 -1 5.30 12.70 -1 22 1 14.30 11.40 -1 22 1 -20.50 10.50 1 -22 -1 -4.40 11.90 0 22 1 21.00 10.30 0 -22 -1 -2.90 10.30 1 22 1 0.90 11.10 -1 -22 -1 8.70 11.30 2 22 1 4.20 11.80 -2 -22 -1 26.80 14.60 -2 22 2 -1.40 13.60 -2 22 2 -8.60 11.20 2 -22 -2 12.80 13.10 -1 22 2 6.70 10.10 -1 22 2 11.60 11.50 1 -22 -2 -3.90 11.40 0 22 2 -24.60 9.60 0 22 2 3.50 10.60 0 -22 -2 0.40 11.80 1 22 2 -4.90 10.40 -1 -22 -2 -12.70 10.60 2 22 2 14.40 12.40 -2 -22 -2 13.50 13.10 -2 22 3 8.10 14.00 -2 22 3 9.80 10.50 2 -22 -3 4.90 12.30 -1 22 3 -26.80 11.90 -1 22 3 22.70 10.10 1 -22 -3 5.10 12.40 0 22 3 20.60 10.50 0 -22 -3 -1.60 10.20 1 22 3 -7.50 10.80 -1 -22 -3 -2.50 12.80 -2 22 4 -8.80 10.10 -2 22 4 -12.70 14.40 2 -22 -4 -14.80 12.80 -1 22 4 0.20 12.20 -1 22 4 6.70 11.20 1 -22 -4 -0.40 12.50 0 22 4 -6.70 11.90 0 -22 -4 33.80 13.40 1 22 4 9.50 11.50 -1 -22 -4 -2.70 13.50 -1 22 5 -16.90 11.70 -1 22 5 8.00 14.00 1 -22 -5 -5.10 11.80 0 22 5 5.80 13.20 0 -22 -5 4.60 11.80 0 23 -1 0.90 12.00 0 23 -1 -2.20 10.90 0 -23 1 -9.50 12.10 0 23 0 0.70 11.10 0 23 0 27.60 12.00 0 -23 0 15.60 12.70 0 23 1 -13.40 12.40 0 -23 -1 -12.60 13.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65366 _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 0.53675(11) 0.32828(5) 0.75426(5) 0.0685(3) Uani 1 1 d . . . . . O1 O 1.1224(2) 0.36471(14) 0.58780(14) 0.0767(6) Uani 1 1 d . . . . . C1 C 0.7877(4) 0.33360(15) 0.81828(17) 0.0545(6) Uani 1 1 d . . . . . H1 H 0.829592 0.327975 0.887721 0.065 Uiso 1 1 calc R U . . . C2 C 0.9221(4) 0.34741(15) 0.75368(18) 0.0566(7) Uani 1 1 d . . . . . H2 H 1.067183 0.351865 0.774776 0.068 Uiso 1 1 calc R U . . . C3 C 0.8170(3) 0.35409(12) 0.65208(16) 0.0424(5) Uani 1 1 d . . . . . C4 C 0.6056(4) 0.34552(14) 0.64252(18) 0.0508(6) Uani 1 1 d . . . . . H4 H 0.509911 0.348779 0.581479 0.061 Uiso 1 1 calc R U . . . C5 C 0.9308(3) 0.36595(14) 0.56985(17) 0.0475(6) Uani 1 1 d . . . . . C6 C 0.8162(3) 0.37913(13) 0.46414(16) 0.0441(5) Uani 1 1 d . . . . . C7 C 0.9285(4) 0.39123(19) 0.37630(19) 0.0665(7) Uani 1 1 d . . . . . H7A H 1.002053 0.347939 0.356811 0.080 Uiso 1 1 calc R U . . . H7B H 1.008138 0.437538 0.377848 0.080 Uiso 1 1 calc R U . . . C8 C 0.6906(3) 0.39658(13) 0.32842(16) 0.0439(5) Uani 1 1 d . . . . . C9 C 0.6692(4) 0.44496(15) 0.42147(17) 0.0604(7) Uani 1 1 d . . . . . H9A H 0.733513 0.494409 0.425497 0.072 Uiso 1 1 calc R U . . . H9B H 0.531561 0.445098 0.439134 0.072 Uiso 1 1 calc R U . . . C10 C 0.6628(4) 0.32720(15) 0.39317(17) 0.0590(7) Uani 1 1 d . . . . . H10A H 0.524745 0.320928 0.409215 0.071 Uiso 1 1 calc R U . . . H10B H 0.721594 0.280440 0.374367 0.071 Uiso 1 1 calc R U . . . C11 C 0.5951(4) 0.41140(13) 0.21882(16) 0.0481(6) Uani 1 1 d . . . . . C12 C 0.6401(5) 0.34442(15) 0.15583(18) 0.0642(7) Uani 1 1 d . . . . . H12A H 0.790552 0.341272 0.159096 0.077 Uiso 1 1 calc R U . . . H12B H 0.596799 0.298642 0.184896 0.077 Uiso 1 1 calc R U . . . C13 C 0.5282(6) 0.34915(18) 0.0457(2) 0.0824(10) Uani 1 1 d . . . . . H13A H 0.584529 0.391046 0.013692 0.099 Uiso 1 1 calc R U . . . H13B H 0.554097 0.303426 0.011099 0.099 Uiso 1 1 calc R U . . . C14 C 0.2976(7) 0.3594(2) 0.0367(2) 0.0985(12) Uani 1 1 d . . . . . H14A H 0.239041 0.314575 0.061165 0.118 Uiso 1 1 calc R U . . . H14B H 0.232161 0.365632 -0.033867 0.118 Uiso 1 1 calc R U . . . C15 C 0.2463(5) 0.4265(2) 0.0951(2) 0.0940(12) Uani 1 1 d . . . . . H15A H 0.095436 0.428960 0.090875 0.113 Uiso 1 1 calc R U . . . H15B H 0.289204 0.472115 0.065433 0.113 Uiso 1 1 calc R U . . . C16 C 0.3574(4) 0.4220(2) 0.20539(19) 0.0746(9) Uani 1 1 d . . . . . H16A H 0.299491 0.380255 0.237091 0.090 Uiso 1 1 calc R U . . . H16B H 0.329836 0.467745 0.239482 0.090 Uiso 1 1 calc R U . . . C17 C 0.6998(5) 0.48253(16) 0.1875(2) 0.0722(8) Uani 1 1 d . . . . . H17A H 0.673117 0.524113 0.228347 0.108 Uiso 1 1 calc R U . . . H17B H 0.642930 0.493381 0.117854 0.108 Uiso 1 1 calc R U . . . H17C H 0.848788 0.474580 0.196622 0.108 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 0.0515(4) 0.0955(6) 0.0623(4) 0.0105(4) 0.0206(3) 0.0031(4) O1 0.0328(9) 0.1350(19) 0.0615(12) 0.0080(11) 0.0074(8) -0.0056(10) C1 0.0517(14) 0.0758(17) 0.0351(12) 0.0093(11) 0.0070(10) 0.0150(12) C2 0.0406(13) 0.0779(18) 0.0480(14) -0.0009(12) 0.0011(11) 0.0034(12) C3 0.0372(11) 0.0468(13) 0.0427(12) -0.0032(9) 0.0066(9) 0.0001(9) C4 0.0401(12) 0.0675(16) 0.0442(13) 0.0008(11) 0.0075(10) -0.0006(11) C5 0.0360(12) 0.0580(15) 0.0481(13) -0.0041(11) 0.0073(10) -0.0043(10) C6 0.0381(11) 0.0548(14) 0.0407(12) -0.0020(10) 0.0107(9) -0.0019(10) C7 0.0503(15) 0.097(2) 0.0547(15) 0.0021(14) 0.0170(12) -0.0010(14) C8 0.0463(12) 0.0484(13) 0.0392(12) -0.0014(9) 0.0136(10) 0.0003(10) C9 0.0742(17) 0.0632(16) 0.0443(13) -0.0057(12) 0.0132(12) 0.0080(13) C10 0.0707(17) 0.0600(16) 0.0423(13) 0.0037(11) 0.0022(12) -0.0127(13) C11 0.0548(14) 0.0542(14) 0.0384(12) 0.0036(10) 0.0166(11) 0.0007(11) C12 0.089(2) 0.0619(17) 0.0438(14) -0.0009(12) 0.0193(13) 0.0015(14) C13 0.130(3) 0.076(2) 0.0437(15) -0.0037(14) 0.0242(17) -0.0041(19) C14 0.118(3) 0.123(3) 0.0465(17) 0.0090(18) -0.0035(18) -0.033(2) C15 0.0663(19) 0.160(4) 0.0534(18) 0.026(2) 0.0066(15) 0.012(2) C16 0.0611(17) 0.121(3) 0.0433(14) 0.0118(15) 0.0151(13) 0.0140(17) C17 0.094(2) 0.0636(18) 0.0629(17) 0.0098(14) 0.0256(16) -0.0054(15) 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' 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 C1 S1 C4 92.72(11) . . ? S1 C1 H1 124.7 . . ? C2 C1 S1 110.70(17) . . ? C2 C1 H1 124.7 . . ? C1 C2 H2 123.5 . . ? C1 C2 C3 113.0(2) . . ? C3 C2 H2 123.5 . . ? C2 C3 C5 122.2(2) . . ? C4 C3 C2 111.3(2) . . ? C4 C3 C5 126.5(2) . . ? S1 C4 H4 123.9 . . ? C3 C4 S1 112.29(18) . . ? C3 C4 H4 123.9 . . ? O1 C5 C3 119.7(2) . . ? O1 C5 C6 119.0(2) . . ? C3 C5 C6 121.33(19) . . ? C5 C6 C7 123.00(19) . . ? C5 C6 C8 175.92(18) . . ? C5 C6 C9 128.9(2) . . ? C5 C6 C10 129.6(2) . . ? C7 C6 C8 52.93(13) . . ? C7 C6 C9 87.59(19) . . ? C7 C6 C10 87.05(19) . . ? C9 C6 C8 52.90(13) . . ? C10 C6 C8 52.56(13) . . ? C10 C6 C9 87.05(18) . . ? C6 C7 H7A 116.0 . . ? C6 C7 H7B 116.0 . . ? C6 C7 C8 75.15(16) . . ? H7A C7 H7B 113.0 . . ? C8 C7 H7A 116.0 . . ? C8 C7 H7B 116.0 . . ? C7 C8 C6 51.92(13) . . ? C7 C8 C9 86.54(18) . . ? C9 C8 C6 52.48(13) . . ? C10 C8 C6 52.44(13) . . ? C10 C8 C7 86.23(19) . . ? C10 C8 C9 86.66(18) . . ? C11 C8 C6 178.48(19) . . ? C11 C8 C7 126.63(19) . . ? C11 C8 C9 127.8(2) . . ? C11 C8 C10 128.67(19) . . ? C6 C9 C8 74.62(16) . . ? C6 C9 H9A 116.0 . . ? C6 C9 H9B 116.0 . . ? C8 C9 H9A 116.0 . . ? C8 C9 H9B 116.0 . . ? H9A C9 H9B 113.0 . . ? C6 C10 C8 75.00(16) . . ? C6 C10 H10A 116.0 . . ? C6 C10 H10B 116.0 . . ? C8 C10 H10A 116.0 . . ? C8 C10 H10B 116.0 . . ? H10A C10 H10B 113.0 . . ? C8 C11 C12 109.02(19) . . ? C8 C11 C16 109.98(18) . . ? C8 C11 C17 107.4(2) . . ? C12 C11 C16 109.4(2) . . ? C12 C11 C17 110.0(2) . . ? C16 C11 C17 111.0(2) . . ? C11 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C13 C12 C11 113.4(2) . . ? C13 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C12 C13 H13A 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C14 C13 C12 111.1(3) . . ? C14 C13 H13A 109.4 . . ? C14 C13 H13B 109.4 . . ? C13 C14 H14A 109.1 . . ? C13 C14 H14B 109.1 . . ? C13 C14 C15 112.3(3) . . ? H14A C14 H14B 107.9 . . ? C15 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C14 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C14 C15 C16 111.2(3) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C11 C16 H16A 109.0 . . ? C11 C16 H16B 109.0 . . ? C15 C16 C11 112.9(2) . . ? C15 C16 H16A 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 S1 C1 1.686(3) . ? S1 C4 1.690(2) . ? O1 C5 1.218(3) . ? C1 H1 0.9300 . ? C1 C2 1.377(3) . ? C2 H2 0.9300 . ? C2 C3 1.412(3) . ? C3 C4 1.360(3) . ? C3 C5 1.471(3) . ? C4 H4 0.9300 . ? C5 C6 1.492(3) . ? C6 C7 1.531(3) . ? C6 C8 1.880(3) . ? C6 C9 1.546(3) . ? C6 C10 1.543(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.552(3) . ? C8 C9 1.555(3) . ? C8 C10 1.545(3) . ? C8 C11 1.511(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.527(3) . ? C11 C16 1.528(3) . ? C11 C17 1.535(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.523(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.488(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.506(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.524(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? 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 S1 C1 C2 C3 0.5(3) . . . . ? O1 C5 C6 C7 0.0(4) . . . . ? O1 C5 C6 C9 -117.3(3) . . . . ? O1 C5 C6 C10 117.2(3) . . . . ? C1 S1 C4 C3 1.1(2) . . . . ? C1 C2 C3 C4 0.3(3) . . . . ? C1 C2 C3 C5 -177.6(2) . . . . ? C2 C3 C4 S1 -0.9(3) . . . . ? C2 C3 C5 O1 5.4(4) . . . . ? C2 C3 C5 C6 -174.9(2) . . . . ? C3 C5 C6 C7 -179.6(2) . . . . ? C3 C5 C6 C9 63.1(3) . . . . ? C3 C5 C6 C10 -62.4(3) . . . . ? C4 S1 C1 C2 -0.9(2) . . . . ? C4 C3 C5 O1 -172.1(3) . . . . ? C4 C3 C5 C6 7.5(4) . . . . ? C5 C3 C4 S1 176.82(19) . . . . ? C5 C6 C7 C8 -179.7(2) . . . . ? C5 C6 C9 C8 175.3(2) . . . . ? C5 C6 C10 C8 -175.6(2) . . . . ? C6 C7 C8 C9 43.30(18) . . . . ? C6 C7 C8 C10 -43.58(18) . . . . ? C6 C7 C8 C11 179.4(2) . . . . ? C7 C6 C8 C9 -120.3(2) . . . . ? C7 C6 C8 C10 119.8(2) . . . . ? C7 C6 C9 C8 43.57(17) . . . . ? C7 C6 C10 C8 -43.89(17) . . . . ? C7 C8 C9 C6 -42.89(17) . . . . ? C7 C8 C10 C6 43.19(17) . . . . ? C7 C8 C11 C12 67.1(3) . . . . ? C7 C8 C11 C16 -173.0(3) . . . . ? C7 C8 C11 C17 -52.1(3) . . . . ? C8 C11 C12 C13 173.0(2) . . . . ? C8 C11 C16 C15 -172.2(3) . . . . ? C9 C6 C7 C8 -43.55(17) . . . . ? C9 C6 C8 C7 120.3(2) . . . . ? C9 C6 C8 C10 -119.9(2) . . . . ? C9 C6 C10 C8 43.84(16) . . . . ? C9 C8 C10 C6 -43.56(17) . . . . ? C9 C8 C11 C12 -174.1(2) . . . . ? C9 C8 C11 C16 -54.1(3) . . . . ? C9 C8 C11 C17 66.7(3) . . . . ? C10 C6 C7 C8 43.61(17) . . . . ? C10 C6 C8 C7 -119.8(2) . . . . ? C10 C6 C8 C9 119.9(2) . . . . ? C10 C6 C9 C8 -43.59(16) . . . . ? C10 C8 C9 C6 43.53(16) . . . . ? C10 C8 C11 C12 -52.3(3) . . . . ? C10 C8 C11 C16 67.7(3) . . . . ? C10 C8 C11 C17 -171.4(2) . . . . ? C11 C8 C9 C6 -178.1(2) . . . . ? C11 C8 C10 C6 178.7(2) . . . . ? C11 C12 C13 C14 -54.7(4) . . . . ? C12 C11 C16 C15 -52.5(3) . . . . ? C12 C13 C14 C15 55.0(4) . . . . ? C13 C14 C15 C16 -55.1(4) . . . . ? C14 C15 C16 C11 54.3(4) . . . . ? C16 C11 C12 C13 52.7(3) . . . . ? C17 C11 C12 C13 -69.5(3) . . . . ? C17 C11 C16 C15 69.1(3) . . . . ?