#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:17:48 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242494 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132524.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_4132524 loop_ _publ_author_name 'Gr\'elaud, Simon' 'Cooper, Phillippa' 'Feron, Lyman J.' 'Bower, John F.' _publ_section_title ; Branch-Selective and Enantioselective Iridium-Catalyzed Alkene Hydroarylation via Anilide-Directed C-H Oxidative Addition. ; _journal_issue 30 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 9351 _journal_page_last 9356 _journal_paper_doi 10.1021/jacs.8b04627 _journal_volume 140 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C16 H19 N O S' _chemical_formula_sum 'C16 H19 N O S' _chemical_formula_weight 273.38 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2018-02-19 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.05680(10) _cell_length_b 16.3847(4) _cell_length_c 17.2832(4) _cell_measurement_reflns_used 7852 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.84 _cell_measurement_theta_min 2.36 _cell_volume 1431.98(6) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_collection 'Bruker Apex suite' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker area detector' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device 'Bruker Apex II kappa CCD area detector' _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 0.0438 _diffrn_reflns_av_unetI/netI 0.0260 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26937 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.071 _diffrn_reflns_theta_min 1.713 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0786 before and 0.0523 after correction. The Ratio of minimum to maximum transmission is 0.7830. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.268 _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.451 _exptl_crystal_size_mid 0.315 _exptl_crystal_size_min 0.262 _refine_diff_density_max 0.240 _refine_diff_density_min -0.150 _refine_diff_density_rms 0.037 _refine_ls_abs_structure_details ; Flack x determined using 1269 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 179 _refine_ls_number_reflns 3473 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.1122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.0700 _reflns_Friedel_coverage 0.705 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 3213 _reflns_number_total 3473 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04627_si_003.cif _cod_data_source_block testo1 _cod_database_code 4132524 _shelx_shelxl_version_number 2017/1 _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 At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C5(H5), C14(H14) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12) 2.c Idealised Me refined as rotating group: C6(H6A,H6B,H6C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C) ; _shelx_res_file ; TITL testo1_a.res in P2(1)2(1)2(1) testo1.res created by SHELXL-2017/1 at 14:57:22 on 19-Feb-2018 REM Old TITL testo1 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.079, Rweak 0.018, Alpha 0.002, Orientation as input REM Flack x = 0.006 ( 0.027 ) from Parsons' quotients REM Formula found by SHELXT: C16 N O S CELL 0.71073 5.0568 16.3847 17.2832 90 90 90 ZERR 4 0.0001 0.0004 0.0004 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S UNIT 64 76 4 4 4 L.S. 4 PLAN 5 TEMP -173.14 list 4 fmap 2 ACTA REM REM REM WGHT 0.041000 0.112200 FVAR 0.55094 S1 5 0.653115 0.604756 0.503920 11.00000 0.02331 0.02220 = 0.01486 0.00153 0.00140 -0.00131 O1 4 1.027234 0.678893 0.763135 11.00000 0.01203 0.02898 = 0.02284 -0.00201 -0.00003 -0.00007 N1 3 0.603190 0.665354 0.722639 11.00000 0.01070 0.02051 = 0.01646 0.00010 0.00256 0.00020 C1 1 0.536791 0.597912 0.597883 11.00000 0.01576 0.01797 = 0.01533 0.00268 0.00121 0.00242 C2 1 0.663156 0.654896 0.643194 11.00000 0.01373 0.01639 = 0.01675 0.00149 -0.00009 0.00348 C3 1 0.852861 0.702544 0.602675 11.00000 0.01694 0.01716 = 0.02020 0.00341 -0.00022 0.00044 AFIX 43 H3 2 0.956220 0.744222 0.626035 11.00000 -1.20000 AFIX 0 C4 1 0.869637 0.681671 0.526567 11.00000 0.02003 0.02100 = 0.02099 0.00601 0.00207 -0.00141 AFIX 43 H4 2 0.986496 0.706568 0.490578 11.00000 -1.20000 AFIX 0 C5 1 0.325944 0.537287 0.620458 11.00000 0.01663 0.01899 = 0.01893 0.00085 0.00075 0.00039 AFIX 13 H5 2 0.167073 0.569061 0.637182 11.00000 -1.20000 AFIX 0 C6 1 0.242975 0.484268 0.551525 11.00000 0.02310 0.02443 = 0.02072 -0.00009 -0.00338 -0.00299 AFIX 137 H6A 2 0.182143 0.519373 0.509207 11.00000 -1.50000 H6B 2 0.099336 0.447714 0.567273 11.00000 -1.50000 H6C 2 0.394405 0.451825 0.534028 11.00000 -1.50000 AFIX 0 C7 1 0.406994 0.482706 0.687978 11.00000 0.01897 0.01758 = 0.01734 0.00032 -0.00088 -0.00471 C8 1 0.618492 0.429149 0.681400 11.00000 0.02132 0.03604 = 0.02691 0.00873 0.00601 0.00519 AFIX 43 H8 2 0.723718 0.429957 0.635871 11.00000 -1.20000 AFIX 0 C9 1 0.679173 0.374401 0.740131 11.00000 0.02792 0.03230 = 0.03555 0.00929 -0.00283 0.00396 AFIX 43 H9 2 0.823610 0.337829 0.734353 11.00000 -1.20000 AFIX 0 C10 1 0.529440 0.373172 0.806903 11.00000 0.04122 0.02277 = 0.02238 0.00709 -0.00970 -0.00784 AFIX 43 H10 2 0.570118 0.335827 0.847230 11.00000 -1.20000 AFIX 0 C11 1 0.320823 0.426462 0.814586 11.00000 0.04722 0.03496 = 0.01850 0.00195 0.00861 -0.00492 AFIX 43 H11 2 0.217986 0.426018 0.860584 11.00000 -1.20000 AFIX 0 C12 1 0.258919 0.481201 0.755357 11.00000 0.03261 0.02453 = 0.02168 -0.00163 0.00650 0.00076 AFIX 43 H12 2 0.114250 0.517650 0.761333 11.00000 -1.20000 AFIX 0 C13 1 0.789265 0.677174 0.777703 11.00000 0.01560 0.01418 = 0.01838 0.00085 -0.00028 0.00126 C14 1 0.686420 0.685395 0.859753 11.00000 0.01539 0.02969 = 0.01805 -0.00075 0.00177 -0.00085 AFIX 13 H14 2 0.490163 0.692735 0.858315 11.00000 -1.20000 AFIX 0 C15 1 0.751609 0.606753 0.903241 11.00000 0.05403 0.04334 = 0.02698 0.01338 0.00629 -0.00315 AFIX 137 H15A 2 0.676463 0.560072 0.875433 11.00000 -1.50000 H15B 2 0.676222 0.609270 0.955423 11.00000 -1.50000 H15C 2 0.943958 0.600470 0.906763 11.00000 -1.50000 AFIX 0 C16 1 0.811769 0.759445 0.898622 11.00000 0.04076 0.04239 = 0.02516 -0.01360 0.00395 -0.00602 AFIX 137 H16A 2 1.004619 0.753541 0.898391 11.00000 -1.50000 H16B 2 0.748871 0.763395 0.952124 11.00000 -1.50000 H16C 2 0.762378 0.808988 0.870331 11.00000 -1.50000 AFIX 0 H1 2 0.454731 0.664887 0.736136 11.00000 0.03530 HKLF 4 REM testo1_a.res in P2(1)2(1)2(1) REM R1 = 0.0284 for 3213 Fo > 4sig(Fo) and 0.0322 for all 3473 data REM 179 parameters refined using 0 restraints END WGHT 0.0410 0.1122 REM Highest difference peak 0.240, deepest hole -0.150, 1-sigma level 0.037 Q1 1 0.7456 0.6792 0.8202 11.00000 0.05 0.24 Q2 1 0.5684 0.6042 0.5535 11.00000 0.05 0.21 Q3 1 0.3409 0.4794 0.7223 11.00000 0.05 0.20 Q4 1 0.7710 0.6746 0.6220 11.00000 0.05 0.20 Q5 1 0.4731 0.4419 0.6783 11.00000 0.05 0.20 ; _shelx_res_checksum 26224 _shelx_hkl_file ; -1 0 0 0.90 0.70 -1 0 0 0.20 0.80 -1 0 0 -0.80 0.60 1 0 0 0.20 0.50 1 0 0 0.60 0.50 -1 0 0 1.30 0.50 -1 0 0 0.70 0.50 -2 0 0 1204.28 28.10 2 0 0 1239.28 28.20 2 0 0 1227.58 28.20 -2 0 0 1194.08 29.20 -2 0 0 1222.68 29.20 -2 0 0 1184.18 28.20 -2 0 0 1177.98 29.60 -3 0 0 1.20 1.50 -3 0 0 0.10 1.00 -3 0 0 -0.50 1.30 -3 0 0 -1.90 1.40 -3 0 0 -0.40 0.50 3 0 0 -1.00 0.80 3 0 0 -0.10 0.80 -4 0 0 119.39 6.30 -4 0 0 115.69 7.10 -4 0 0 116.29 6.30 -4 0 0 120.99 4.60 4 0 0 122.89 4.50 -5 0 0 0.50 2.10 -5 0 0 -1.10 2.80 -5 0 0 -1.10 1.90 -6 0 0 140.79 9.60 -6 0 0 108.49 7.90 0 -1 0 0.20 0.10 0 1 0 0.00 0.10 0 -1 0 -0.10 0.10 0 -1 0 0.00 0.10 0 -1 0 0.00 0.10 0 1 0 0.10 0.10 0 1 0 0.00 0.10 -1 1 0 369.16 9.10 -1 -1 0 371.46 9.70 1 -1 0 363.66 9.40 -1 1 0 362.46 9.40 -1 -1 0 389.46 9.80 -1 1 0 374.76 9.60 1 -1 0 388.26 9.50 -1 1 0 367.86 9.40 -1 -1 0 372.76 9.50 1 -1 0 381.46 9.50 -1 1 0 363.56 9.40 -2 1 0 60.29 3.00 -2 1 0 55.09 2.90 2 -1 0 66.49 3.10 -2 -1 0 70.99 3.60 2 1 0 70.89 2.20 -2 1 0 62.39 3.50 2 -1 0 59.29 3.00 -2 1 0 55.49 2.80 2 -1 0 58.69 3.10 -2 1 0 63.79 3.30 2 1 0 63.99 2.10 -2 -1 0 69.29 2.20 -2 -1 0 70.59 3.40 -2 -1 0 69.99 3.70 3 -1 0 173.58 6.00 -3 -1 0 163.48 7.20 -3 -1 0 159.18 4.80 -3 -1 0 184.78 4.90 -3 1 0 174.78 5.80 -3 -1 0 167.78 6.90 -3 1 0 185.68 7.60 3 1 0 173.98 4.90 3 -1 0 164.98 6.00 -3 1 0 171.78 6.00 3 -1 0 176.08 6.00 -3 1 0 172.78 6.80 3 1 0 158.78 4.70 -3 -1 0 165.78 6.70 -3 1 0 174.98 6.50 -4 1 0 7.20 3.00 -4 -1 0 2.90 2.50 -4 1 0 11.70 2.80 -4 1 0 5.70 2.30 -4 1 0 8.00 1.90 -4 -1 0 10.40 1.20 4 -1 0 7.40 1.60 -4 -1 0 7.40 2.40 -4 -1 0 4.90 2.50 -5 1 0 161.98 7.80 -5 -1 0 150.58 8.00 -5 1 0 140.79 7.80 -5 1 0 158.78 8.90 -5 -1 0 155.18 9.00 -5 -1 0 160.98 8.50 -6 -1 0 6.40 3.10 -6 -1 0 0.20 2.80 -6 1 0 -2.30 2.40 -6 1 0 -1.80 2.50 -6 -1 0 -0.20 2.90 0 -2 0 66.39 2.00 0 2 0 62.59 2.20 0 2 0 64.19 2.20 0 -2 0 63.39 2.30 0 -2 0 61.29 2.20 -1 -2 0 17.90 1.50 -1 -2 0 13.90 0.70 1 2 0 14.60 0.80 -1 -2 0 17.90 1.70 -1 2 0 14.10 1.40 -1 2 0 14.70 1.60 1 -2 0 12.50 1.60 -1 -2 0 17.80 1.80 -1 2 0 12.80 1.50 -1 2 0 12.70 0.90 -1 2 0 10.80 1.40 1 2 0 15.90 0.80 1 -2 0 12.80 1.60 2 -2 0 236.48 7.50 -2 2 0 232.28 6.80 -2 -2 0 242.08 7.50 2 -2 0 250.27 7.60 -2 2 0 227.68 7.30 -2 -2 0 240.98 7.90 -2 2 0 232.68 7.20 -2 2 0 233.98 7.70 -2 2 0 235.08 7.40 -2 -2 0 231.28 7.90 -3 2 0 273.97 8.80 3 -2 0 273.67 8.80 -3 2 0 287.57 10.00 -3 2 0 275.17 8.50 3 -2 0 276.47 8.80 -3 -2 0 255.87 9.80 -3 2 0 266.97 9.10 -3 -2 0 264.07 9.20 -3 2 0 271.97 8.60 -3 -2 0 275.47 9.80 -4 2 0 0.00 2.10 -4 2 0 -0.60 1.60 -4 2 0 0.70 1.80 -4 -2 0 -2.30 2.20 -4 2 0 0.40 1.70 -4 -2 0 -2.60 1.80 4 -2 0 0.30 1.30 -4 -2 0 5.90 2.40 -5 2 0 1.50 1.80 -5 2 0 3.20 2.10 -5 -2 0 7.20 2.60 -5 -2 0 1.30 2.60 -5 2 0 0.00 2.70 5 -2 0 2.20 1.40 -5 2 0 0.30 2.00 -5 -2 0 3.10 2.90 -6 -2 0 25.00 4.80 -6 2 0 24.40 5.20 -6 -2 0 29.30 5.50 -6 -2 0 27.40 4.80 -6 2 0 20.50 4.20 0 3 0 0.70 0.60 0 3 0 -0.30 0.70 0 -3 0 0.80 0.60 0 -3 0 -0.60 0.70 0 -3 0 0.20 0.70 1 3 0 9999.00 217.28 -1 3 0 9518.85 222.88 -1 3 0 9696.63 220.78 1 -3 0 9731.93 222.88 1 3 0 9522.95 217.28 -1 -3 0 9660.73 221.18 -1 3 0 9534.45 223.88 -1 -3 0 9415.36 216.88 -1 -3 0 9269.37 218.98 -1 -3 0 9482.45 216.88 -1 -3 0 9228.28 222.48 1 -3 0 9704.63 223.58 2 -3 0 674.03 17.50 -2 3 0 645.44 17.20 -2 3 0 644.34 17.20 2 -3 0 652.93 17.40 -2 -3 0 671.83 17.70 -2 3 0 664.03 17.20 -2 -3 0 666.63 17.00 -2 3 0 647.74 17.00 -2 3 0 648.54 15.90 -2 -3 0 644.34 17.60 -3 3 0 3.70 1.70 -3 3 0 -1.30 1.20 3 -3 0 0.40 1.70 -3 -3 0 0.50 1.40 -3 -3 0 2.00 1.90 -3 3 0 -0.10 1.30 -3 3 0 0.60 1.10 -3 3 0 0.50 1.70 -3 -3 0 2.20 2.10 3 -3 0 -0.90 1.30 -4 3 0 72.49 4.80 -4 3 0 73.19 5.60 4 -3 0 73.39 4.60 -4 3 0 78.09 4.40 -4 -3 0 71.59 5.80 -4 -3 0 69.49 5.00 -4 3 0 74.49 5.10 -4 -3 0 71.99 5.70 -5 3 0 84.79 5.20 -5 -3 0 73.69 6.40 -5 -3 0 93.49 7.00 -5 3 0 87.29 6.40 -5 3 0 85.69 7.60 5 -3 0 91.49 5.20 -5 -3 0 91.39 8.20 -6 3 0 9.30 4.00 -6 3 0 8.30 3.30 -6 -3 0 5.70 4.00 -6 -3 0 11.70 3.90 -6 -3 0 6.50 3.60 0 -4 0 1608.54 36.80 0 -4 0 1533.15 36.70 0 4 0 1570.44 36.70 0 -4 0 1555.24 36.00 0 4 0 1539.25 36.60 1 4 0 167.78 5.10 -1 -4 0 166.98 5.10 -1 -4 0 168.58 5.00 1 -4 0 178.58 6.20 -1 4 0 179.78 5.20 1 4 0 169.08 5.00 -1 4 0 177.98 6.20 1 4 0 170.18 5.10 -1 -4 0 167.58 5.90 -1 -4 0 176.88 5.80 -1 4 0 177.98 6.10 1 -4 0 177.08 6.40 -1 -4 0 160.48 5.40 2 -4 0 88.69 4.70 -2 -4 0 89.29 4.70 -2 4 0 73.39 4.20 -2 4 0 89.19 4.40 2 -4 0 84.59 4.60 -2 4 0 85.49 4.20 -2 -4 0 85.79 4.00 -2 -4 0 81.59 4.50 -3 -4 0 18.40 3.10 -3 4 0 18.90 2.60 -3 4 0 20.50 2.00 -3 -4 0 18.80 3.20 3 -4 0 17.80 2.70 -3 4 0 20.00 2.80 -3 4 0 21.50 3.00 3 -4 0 22.90 3.20 -3 4 0 20.40 3.00 -3 -4 0 26.30 3.10 4 -4 0 77.29 5.20 -4 4 0 76.19 5.70 -4 4 0 79.29 5.30 -4 -4 0 88.39 5.50 -4 -4 0 81.99 6.30 -4 4 0 75.09 4.20 -4 -4 0 74.99 6.20 -4 4 0 81.09 5.30 5 -4 0 36.40 4.00 -5 -4 0 49.70 6.10 -5 4 0 45.80 5.70 -5 4 0 36.40 4.90 -5 -4 0 37.50 5.00 -5 4 0 38.30 4.20 -5 -4 0 55.89 6.20 -6 -4 0 89.99 8.90 -6 -4 0 99.59 8.00 -6 -4 0 91.39 7.10 -6 4 0 82.49 7.60 -6 4 0 88.59 8.40 0 -5 0 -0.10 1.30 0 5 0 0.30 1.20 0 -5 0 0.70 1.40 0 5 0 1.30 1.30 0 -5 0 -0.90 1.00 -1 5 0 1054.89 27.00 -1 5 0 1101.49 25.50 -1 -5 0 1079.29 26.00 1 5 0 1089.89 25.90 -1 5 0 1091.59 27.10 1 -5 0 1085.39 24.60 1 -5 0 1061.99 27.40 -1 -5 0 1092.89 26.80 -1 -5 0 1089.89 25.80 1 5 0 1095.19 25.80 1 -5 0 1082.29 27.20 2 5 0 200.78 5.60 -2 5 0 200.38 7.10 -2 5 0 212.98 7.70 -2 -5 0 205.38 5.60 2 -5 0 220.08 8.20 -2 -5 0 206.98 7.20 -2 -5 0 200.98 7.80 2 5 0 217.38 5.50 2 -5 0 210.08 8.00 -2 -5 0 201.58 7.60 -2 5 0 216.58 7.80 3 -5 0 11.80 2.90 3 -5 0 13.70 2.80 -3 5 0 15.50 2.50 -3 -5 0 12.70 3.00 -3 5 0 13.50 2.50 -3 -5 0 8.80 2.30 -3 5 0 14.20 2.60 -3 -5 0 7.60 2.90 -3 5 0 13.60 2.80 4 -5 0 13.90 3.00 -4 -5 0 14.50 3.10 -4 5 0 10.50 2.60 -4 -5 0 12.10 3.40 -4 5 0 3.50 2.40 -4 5 0 14.40 3.10 -4 -5 0 9.00 3.30 -5 -5 0 16.00 3.50 -5 5 0 18.50 4.20 -5 -5 0 13.80 3.80 -5 5 0 16.20 3.40 -5 5 0 19.50 3.70 5 -5 0 16.40 3.20 -5 -5 0 14.90 3.90 -6 5 0 2.70 3.10 -6 -5 0 0.40 2.80 -6 5 0 10.30 4.00 -6 -5 0 2.70 3.80 -6 -5 0 6.50 3.90 0 6 0 369.06 11.00 0 -6 0 385.16 11.30 0 -6 0 380.76 10.20 0 6 0 383.66 11.10 0 -6 0 374.06 11.30 1 -6 0 383.86 12.30 -1 -6 0 409.16 11.00 -1 -6 0 410.26 11.20 1 -6 0 395.06 12.20 1 6 0 416.66 11.10 -1 6 0 412.86 10.30 1 6 0 399.66 11.00 -1 -6 0 407.36 11.80 -1 6 0 388.16 12.00 1 -6 0 391.76 9.60 -1 6 0 398.06 12.00 -2 -6 0 3.90 1.80 -2 -6 0 1.90 2.10 -2 -6 0 0.40 0.50 2 6 0 4.30 1.00 -2 -6 0 0.60 0.50 -2 -6 0 3.90 1.50 2 -6 0 -0.20 1.70 2 6 0 4.80 1.10 -2 6 0 0.50 1.60 -2 6 0 2.90 1.60 2 -6 0 1.00 2.10 -2 -6 0 1.80 1.00 3 -6 0 115.39 6.70 -3 -6 0 101.49 6.10 3 -6 0 100.09 6.20 -3 6 0 99.59 5.80 -3 6 0 103.79 6.10 -3 6 0 97.59 5.40 -3 -6 0 104.99 6.60 -3 -6 0 94.59 5.60 4 -6 0 19.10 3.50 -4 6 0 21.90 3.80 -4 -6 0 27.90 4.60 -4 -6 0 25.40 4.30 -4 6 0 26.20 3.90 -4 6 0 23.40 3.50 -4 -6 0 25.20 3.70 -5 -6 0 20.40 4.30 -5 -6 0 27.30 4.30 5 -6 0 26.10 4.00 -5 6 0 24.50 3.90 -5 6 0 25.10 4.30 -5 6 0 26.80 4.30 -5 -6 0 25.90 4.80 -6 -6 0 34.90 6.40 6 -6 0 40.40 5.10 -6 6 0 31.20 5.00 -6 -6 0 21.10 4.50 -6 6 0 31.40 5.60 -6 -6 0 34.40 6.20 -6 6 0 33.90 5.00 0 -7 0 1.30 1.50 0 7 0 0.10 1.30 0 -7 0 0.30 1.20 0 7 0 0.90 1.20 0 -7 0 -0.60 1.40 -1 -7 0 13.00 1.90 1 -7 0 8.80 2.30 1 7 0 8.20 1.70 1 -7 0 9.40 1.10 -1 7 0 10.00 1.20 -1 -7 0 10.20 2.30 1 7 0 9.80 1.70 -1 -7 0 11.20 2.00 -1 7 0 12.30 2.40 1 -7 0 5.90 2.10 -1 7 0 10.20 2.20 2 -7 0 73.49 5.10 -2 -7 0 68.49 4.70 2 7 0 67.19 3.40 2 -7 0 73.49 5.20 -2 -7 0 73.59 3.50 -2 7 0 68.69 4.60 -2 -7 0 78.09 5.00 2 7 0 70.19 3.20 -2 7 0 69.59 4.80 -2 -7 0 76.99 3.20 2 7 0 71.59 3.40 -2 -7 0 82.89 4.40 -3 7 0 0.70 2.10 -3 7 0 2.10 2.30 -3 -7 0 1.40 2.00 -3 -7 0 -1.50 2.10 -3 7 0 0.80 1.80 3 -7 0 0.50 2.30 3 -7 0 1.80 2.90 -3 -7 0 0.20 2.70 -4 -7 0 101.59 6.60 -4 7 0 106.79 6.50 -4 7 0 109.79 6.60 -4 -7 0 106.49 7.00 4 -7 0 106.89 7.10 -4 -7 0 105.39 7.50 -4 7 0 101.49 6.70 -5 7 0 8.40 3.20 5 -7 0 2.80 2.30 -5 7 0 2.20 2.50 -5 -7 0 2.40 2.70 -5 -7 0 7.40 3.60 -5 7 0 8.30 2.80 -5 -7 0 1.50 2.30 -6 7 0 15.70 4.20 -6 -7 0 18.00 5.20 6 -7 0 16.90 3.80 -6 7 0 27.50 4.60 -6 -7 0 15.30 4.40 -6 -7 0 23.70 5.40 -6 7 0 20.60 5.10 0 -8 0 25.50 2.60 0 8 0 30.40 3.20 0 -8 0 24.00 3.00 0 -8 0 34.00 3.60 0 8 0 33.20 3.40 1 -8 0 74.59 2.80 -1 -8 0 71.59 4.30 -1 -8 0 76.79 4.50 -1 -8 0 77.59 4.10 1 8 0 72.09 4.00 1 8 0 82.09 4.30 1 -8 0 65.39 5.10 -1 8 0 73.29 2.90 -1 8 0 73.39 4.80 -1 8 0 69.09 4.80 1 -8 0 77.39 5.30 -2 -8 0 21.50 2.90 -2 8 0 20.90 3.30 -2 -8 0 24.20 3.50 2 -8 0 21.80 3.70 -2 8 0 19.30 3.20 2 8 0 29.60 2.70 -2 -8 0 23.20 2.50 2 -8 0 27.60 3.90 -2 -8 0 26.00 2.20 2 8 0 27.50 2.60 2 8 0 21.10 2.20 -3 -8 0 10.70 1.10 3 8 0 12.50 1.20 -3 -8 0 7.00 2.50 3 -8 0 9.70 3.20 -3 8 0 6.80 2.70 -3 8 0 12.60 2.70 -3 8 0 8.90 3.10 3 -8 0 8.50 3.30 -3 -8 0 17.30 3.70 -3 -8 0 8.90 3.10 -4 8 0 12.50 3.10 -4 8 0 11.00 3.30 -4 8 0 11.40 2.80 -4 -8 0 11.50 3.80 -4 -8 0 4.70 3.00 -4 -8 0 9.80 3.00 4 -8 0 10.30 3.30 -5 8 0 5.00 2.90 -5 -8 0 6.50 3.50 -5 8 0 4.80 2.70 -5 -8 0 8.00 3.90 -5 -8 0 3.40 2.70 5 -8 0 8.20 3.10 -5 8 0 7.40 3.30 -6 -8 0 4.30 4.20 -6 -8 0 1.50 3.90 -6 -8 0 -0.20 3.20 -6 8 0 -1.40 2.90 -6 8 0 2.60 3.10 6 -8 0 5.10 2.80 -6 8 0 2.70 3.00 0 9 0 0.10 1.70 0 -9 0 3.30 2.10 0 -9 0 -1.50 1.70 0 9 0 -0.30 1.50 0 -9 0 -1.00 1.40 1 9 0 2.80 1.60 -1 9 0 2.30 2.10 1 -9 0 3.90 2.60 -1 -9 0 3.20 1.90 1 -9 0 3.70 1.10 -1 9 0 5.40 2.30 1 -9 0 1.20 2.60 -1 -9 0 3.60 2.00 -1 -9 0 1.60 1.40 1 9 0 3.30 1.60 -2 -9 0 8.00 2.10 -2 9 0 7.40 2.60 -2 -9 0 9.50 1.80 2 9 0 10.70 2.10 2 9 0 9.30 1.80 -2 -9 0 3.40 2.80 -2 9 0 12.60 3.10 2 -9 0 11.40 3.30 2 -9 0 11.10 3.30 3 -9 0 12.60 3.80 3 -9 0 14.90 4.10 -3 -9 0 13.00 3.10 -3 -9 0 13.10 1.60 -3 -9 0 12.00 3.50 -3 9 0 12.40 3.50 -3 9 0 11.30 3.30 3 9 0 13.00 1.50 -3 9 0 14.70 2.80 -3 -9 0 18.20 3.90 -4 -9 0 23.00 3.80 -4 9 0 23.10 3.80 -4 -9 0 18.00 4.20 -4 -9 0 28.50 4.90 4 -9 0 24.70 4.50 -4 9 0 17.00 3.20 -4 9 0 22.70 4.30 -5 9 0 11.70 3.40 -5 9 0 11.40 3.80 5 -9 0 8.80 3.30 -5 -9 0 19.40 4.70 -5 9 0 18.10 4.00 -5 -9 0 13.30 4.60 -5 -9 0 10.40 3.40 -6 9 0 81.19 7.90 -6 9 0 72.79 7.80 -6 -9 0 55.99 7.00 6 -9 0 56.29 6.70 -6 -9 0 68.39 8.50 -6 9 0 61.49 7.30 -6 -9 0 90.49 9.40 0 10 0 571.54 17.40 0 -10 0 615.74 18.30 0 -10 0 594.14 16.10 0 -10 0 576.24 17.80 0 10 0 598.14 17.60 -1 -10 0 9.20 2.20 1 10 0 10.00 2.40 -1 -10 0 4.10 2.30 1 -10 0 8.10 3.10 1 10 0 10.50 2.30 1 -10 0 0.10 2.40 -1 10 0 5.20 2.50 1 -10 0 8.00 1.50 -1 10 0 6.50 2.40 -1 -10 0 8.60 2.60 2 10 0 18.10 2.50 2 -10 0 19.20 4.20 -2 -10 0 18.60 3.80 -2 10 0 27.90 4.30 2 -10 0 19.80 4.40 -2 -10 0 22.10 3.40 -2 -10 0 19.20 3.00 -2 10 0 18.40 3.60 3 -10 0 33.30 5.10 -3 -10 0 31.80 4.20 -3 10 0 31.20 3.80 -3 -10 0 25.10 4.60 -3 -10 0 30.60 2.60 3 -10 0 26.70 4.60 -3 10 0 27.30 4.40 -3 10 0 26.30 4.10 3 10 0 32.10 2.40 -4 -10 0 -0.70 2.50 -4 10 0 4.60 2.50 -4 -10 0 3.30 3.00 4 -10 0 0.90 2.70 -4 10 0 1.00 2.80 -4 -10 0 6.70 3.70 -5 10 0 19.40 4.10 -5 10 0 12.50 4.00 -5 -10 0 14.00 4.30 5 -10 0 16.60 4.10 -5 -10 0 11.70 3.70 -5 10 0 16.00 4.00 -5 -10 0 15.10 4.50 0 11 0 -1.20 2.00 0 -11 0 0.20 2.40 0 -11 0 -1.60 1.70 0 11 0 0.50 1.90 0 -11 0 -2.70 2.20 1 11 0 272.37 10.00 1 -11 0 266.07 8.00 1 -11 0 271.67 11.50 -1 11 0 284.87 11.20 1 -11 0 280.57 11.70 -1 -11 0 287.67 10.40 1 11 0 263.87 9.90 -1 -11 0 273.07 10.60 -1 -11 0 255.37 10.00 -1 11 0 270.57 10.80 2 11 0 19.00 2.70 -2 -11 0 20.60 4.10 2 -11 0 16.50 4.00 2 -11 0 15.90 4.00 -2 11 0 17.80 3.60 -2 11 0 19.30 3.70 -2 -11 0 19.70 3.20 3 -11 0 1.50 3.50 3 11 0 -0.90 1.10 -3 -11 0 1.60 1.60 -3 11 0 -2.40 2.10 -3 11 0 3.00 2.90 -3 11 0 1.30 1.80 3 -11 0 -1.70 2.60 -3 -11 0 -0.40 2.80 -4 -11 0 0.90 3.50 -4 11 0 0.90 2.20 -4 11 0 0.50 2.60 -4 -11 0 1.90 2.70 4 -11 0 -1.70 3.10 4 -11 0 1.90 3.10 -5 -11 0 51.19 6.10 -5 11 0 62.19 6.50 -5 11 0 73.09 7.20 -5 -11 0 44.50 6.60 -5 11 0 71.19 7.80 5 -11 0 56.69 7.00 -5 -11 0 64.99 8.00 0 -12 0 152.18 8.30 0 12 0 153.98 8.00 0 12 0 165.28 8.10 0 -12 0 163.08 6.80 0 -12 0 139.99 8.30 -1 -12 0 0.70 2.80 1 -12 0 2.20 3.60 -1 -12 0 2.20 2.70 1 12 0 4.60 2.40 1 12 0 6.00 2.50 -1 12 0 3.90 2.90 1 -12 0 2.40 3.20 -1 12 0 6.30 3.00 -1 -12 0 7.20 2.70 1 -12 0 3.60 1.60 -2 -12 0 2.70 2.50 -2 12 0 -3.20 2.50 -2 -12 0 1.90 3.10 -2 12 0 -1.10 2.60 2 -12 0 -1.10 3.50 2 12 0 0.90 1.70 2 -12 0 1.40 3.30 -3 12 0 76.29 6.60 -3 -12 0 86.39 6.80 3 12 0 58.39 3.80 3 -12 0 65.49 7.20 -3 -12 0 69.29 4.40 3 -12 0 65.69 7.00 -3 12 0 72.79 6.40 -4 12 0 1.30 2.10 -4 -12 0 -3.20 3.10 4 -12 0 -1.50 3.70 4 -12 0 -1.90 2.60 -4 12 0 -5.50 2.50 -5 -12 0 8.90 4.20 -5 -12 0 4.50 3.40 5 -12 0 4.20 3.70 -5 12 0 4.20 2.80 -5 12 0 3.20 2.90 -5 12 0 6.20 3.70 0 -13 0 2.20 3.40 0 13 0 -1.40 2.20 0 13 0 -0.80 2.30 0 -13 0 -0.90 2.50 0 -13 0 -2.30 2.00 -1 -13 0 186.48 8.90 -1 -13 0 178.78 9.20 -1 13 0 183.98 9.60 1 13 0 183.48 8.60 -1 13 0 189.08 9.40 -1 -13 0 182.68 8.60 1 -13 0 203.48 10.70 1 13 0 172.68 8.50 1 -13 0 180.68 10.10 2 13 0 302.57 11.00 -2 -13 0 325.27 12.70 2 -13 0 289.37 13.70 2 -13 0 306.57 14.10 -2 -13 0 311.07 11.80 -2 13 0 333.77 13.50 -2 13 0 316.17 13.30 -3 13 0 11.80 3.70 3 13 0 13.30 2.30 -3 -13 0 12.70 4.30 -3 -13 0 10.40 2.50 3 -13 0 20.00 4.90 -3 13 0 11.80 3.80 3 -13 0 19.40 4.70 -4 -13 0 2.80 3.50 4 -13 0 6.10 3.60 -4 13 0 10.60 3.10 -4 13 0 7.80 3.70 4 -13 0 5.60 4.00 -5 -13 0 12.00 4.70 -5 13 0 4.50 4.10 -5 13 0 14.70 4.00 5 -13 0 19.30 5.20 -5 13 0 8.30 3.50 0 14 0 700.43 21.40 0 -14 0 691.73 22.00 0 14 0 651.93 20.90 0 -14 0 671.43 19.10 0 -14 0 632.94 21.80 1 -14 0 108.49 8.40 -1 14 0 93.49 7.40 1 14 0 103.49 6.60 -1 -14 0 108.49 7.40 -1 -14 0 93.39 6.50 1 14 0 103.09 6.70 -1 14 0 97.49 7.10 -1 -14 0 101.29 6.90 1 -14 0 96.59 8.30 2 -14 0 18.00 5.10 -2 14 0 20.90 4.70 -2 -14 0 16.50 3.60 -2 14 0 15.40 4.20 2 14 0 18.00 3.10 -2 -14 0 15.10 4.20 2 -14 0 16.80 4.70 -3 14 0 27.60 5.30 3 -14 0 30.10 6.30 -3 -14 0 22.50 3.40 -3 -14 0 30.40 5.60 -3 14 0 26.60 5.00 3 14 0 26.80 3.20 3 -14 0 24.00 5.30 4 -14 0 -2.10 3.00 -4 -14 0 4.60 4.20 4 -14 0 -1.30 3.60 -4 14 0 -0.30 3.00 -4 14 0 1.50 2.30 5 -14 0 0.50 3.40 -5 -14 0 3.90 4.30 -5 14 0 5.90 4.70 -5 14 0 3.10 3.00 -5 14 0 12.80 5.00 0 -15 0 1.60 3.50 0 15 0 0.30 2.70 0 -15 0 0.10 2.30 0 15 0 -0.10 2.40 0 -15 0 -1.70 2.50 -1 -15 0 55.09 5.70 -1 15 0 52.39 6.10 1 -15 0 47.90 6.30 -1 -15 0 40.60 5.60 -1 15 0 43.90 5.60 1 -15 0 38.80 5.80 1 15 0 46.10 5.20 2 -15 0 24.30 5.60 -2 15 0 21.40 4.60 -2 -15 0 14.00 4.20 -2 -15 0 26.00 4.40 2 -15 0 17.60 4.90 -2 15 0 21.00 4.70 2 15 0 15.60 3.10 -3 15 0 1.40 3.30 3 -15 0 -1.10 4.10 -3 -15 0 1.30 2.40 3 15 0 4.10 1.90 -3 -15 0 6.30 4.00 -3 15 0 2.30 3.50 3 -15 0 4.50 3.90 4 -15 0 -2.90 3.60 -4 15 0 5.40 3.70 -4 -15 0 -1.50 3.50 4 -15 0 0.60 3.60 -4 15 0 3.20 2.70 0 16 0 3.70 3.00 0 -16 0 3.00 4.00 0 16 0 -1.30 2.30 0 -16 0 1.90 3.00 1 -16 0 141.39 10.20 1 16 0 134.79 8.10 -1 16 0 145.19 9.20 -1 -16 0 131.29 8.90 1 -16 0 134.49 9.50 -1 -16 0 127.59 7.80 -1 16 0 150.08 9.40 -2 -16 0 -2.00 2.90 -2 16 0 0.70 3.00 -2 16 0 0.10 3.00 2 -16 0 -2.00 3.60 2 16 0 3.00 2.20 -2 -16 0 -3.40 3.00 2 -16 0 -0.50 2.90 -3 -16 0 164.48 10.20 -3 -16 0 162.38 8.30 3 -16 0 163.78 11.40 3 -16 0 162.48 11.50 -3 16 0 165.08 10.70 -3 16 0 182.88 11.20 3 16 0 180.58 7.90 -4 -16 0 8.00 4.40 4 -16 0 4.10 5.20 -4 16 0 11.30 5.00 4 -16 0 9.90 4.80 0 -17 0 -0.20 3.70 0 17 0 2.10 3.10 0 -17 0 1.90 3.20 0 17 0 1.90 2.70 -1 -17 0 43.40 5.30 1 -17 0 49.40 6.80 1 17 0 41.20 5.30 1 -17 0 43.40 6.90 -1 17 0 47.50 6.20 -1 -17 0 41.50 6.10 -1 17 0 38.20 5.80 -2 -17 0 152.48 9.50 -2 17 0 171.78 10.90 -2 -17 0 159.78 9.70 2 17 0 156.48 8.40 -2 17 0 159.88 10.70 2 -17 0 181.98 12.00 2 -17 0 148.59 11.40 3 -17 0 9.80 4.90 -3 17 0 8.20 4.40 3 -17 0 0.30 4.00 -3 17 0 6.60 4.10 3 17 0 10.10 2.70 -3 -17 0 8.90 4.60 -3 -17 0 1.80 2.80 -4 17 0 6.90 4.40 -4 -17 0 8.60 4.50 4 -17 0 1.80 4.60 4 -17 0 3.40 4.20 0 18 0 22.00 4.80 0 -18 0 30.20 5.60 0 -18 0 10.20 4.80 0 18 0 18.80 4.40 -1 18 0 258.67 13.30 1 -18 0 219.38 13.20 1 18 0 262.07 12.10 -1 18 0 251.67 12.80 -1 -18 0 252.57 13.10 -1 -18 0 270.57 11.80 1 -18 0 265.67 14.20 2 18 0 0.90 2.30 2 -18 0 -1.90 3.90 -2 -18 0 3.80 3.70 -2 18 0 6.10 4.00 -2 18 0 5.80 4.00 2 -18 0 2.00 4.00 -2 -18 0 -0.40 3.00 -3 18 0 50.19 7.40 3 -18 0 37.70 7.30 -3 -18 0 62.99 8.10 3 -18 0 39.50 7.50 -3 18 0 43.80 7.30 0 -19 0 3.10 4.30 0 19 0 3.80 3.50 -1 -19 0 109.39 9.30 1 -19 0 133.79 10.60 1 19 0 114.49 8.40 -1 19 0 107.09 9.20 1 -19 0 88.99 9.90 -1 19 0 116.69 9.40 -2 -19 0 4.80 3.80 2 19 0 3.80 2.80 -2 19 0 8.90 4.30 2 -19 0 10.90 5.20 -2 19 0 7.50 4.30 2 -19 0 14.30 6.00 -2 -19 0 5.40 4.20 -3 19 0 2.10 4.40 -3 -19 0 13.70 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15.90 5.00 -1 -3 20 18.70 4.70 2 -3 20 120.99 9.20 -2 3 20 115.79 10.20 2 3 -20 118.89 8.90 2 3 -20 116.29 9.80 -2 -3 -20 115.79 8.40 -2 3 20 116.09 10.00 2 -3 20 125.69 10.70 -2 3 -20 118.89 8.60 2 3 20 104.69 8.80 -2 -3 20 116.09 11.30 2 -3 -20 114.59 9.80 -2 -3 20 122.09 9.70 2 -3 -20 116.39 9.00 -2 -3 20 142.69 10.40 -3 3 20 21.30 5.90 3 3 -20 16.50 5.10 -3 -3 -20 21.10 4.60 3 -3 20 20.90 4.90 -3 3 20 17.50 5.60 -3 3 -20 21.20 4.90 3 -3 -20 20.20 5.50 -3 -3 20 26.80 5.80 -3 3 -20 16.80 4.60 -3 -3 20 25.70 6.30 3 3 20 16.50 4.60 0 -4 -20 32.90 6.30 0 -4 20 39.30 6.30 0 -4 20 33.60 6.30 0 4 20 35.70 6.60 0 -4 -20 29.50 5.30 0 4 20 31.40 6.00 0 4 -20 35.30 5.70 0 4 -20 48.70 7.30 1 4 -20 17.40 4.30 -1 -4 -20 15.90 4.20 -1 4 20 30.00 6.50 1 -4 20 22.90 5.40 1 4 -20 26.40 5.80 1 -4 20 16.80 5.20 -1 4 20 23.00 5.70 -1 -4 -20 16.30 5.00 1 4 20 17.60 4.70 -1 4 -20 32.90 6.30 1 -4 -20 21.10 4.90 -1 -4 20 26.00 5.80 -1 -4 20 24.20 5.30 1 4 20 11.70 4.50 1 -4 -20 22.40 5.50 -2 4 20 2.20 4.60 2 -4 20 3.70 3.80 2 -4 20 8.70 3.70 -2 -4 -20 4.30 3.00 -2 4 20 8.40 4.90 2 4 -20 5.70 3.50 2 4 -20 5.90 4.20 -2 4 20 2.30 4.70 -2 -4 20 7.40 4.80 2 -4 -20 3.30 4.30 -2 -4 20 3.30 4.00 -2 4 -20 0.00 2.90 2 4 20 1.50 3.40 -2 -4 20 5.60 6.20 2 -4 -20 10.30 3.80 -2 4 -20 1.80 2.90 -3 4 20 2.80 5.00 -3 -4 20 11.00 5.10 0 5 -20 6.30 3.30 0 -5 -20 -3.20 3.20 0 5 20 -0.90 3.70 0 -5 20 1.30 3.30 0 -5 20 4.00 4.00 0 5 -20 0.20 3.20 0 -5 -20 -1.70 2.70 0 5 20 3.70 3.90 -1 5 20 152.08 11.50 1 -5 20 165.38 10.80 -1 -5 -20 148.39 9.80 1 5 -20 168.38 11.40 -1 5 20 158.98 11.40 1 -5 20 162.18 10.90 1 5 -20 167.58 10.30 1 5 20 157.98 11.00 1 -5 -20 149.29 9.90 -1 5 -20 144.69 10.70 1 5 20 151.38 10.80 -1 5 -20 149.39 10.10 -1 -5 20 166.98 11.00 -1 -5 20 135.59 11.30 -1 -5 20 149.49 10.30 1 -5 -20 162.38 11.30 2 -5 20 6.30 4.20 -2 5 20 2.10 4.50 2 5 -20 0.50 3.60 -2 5 20 -2.80 5.00 -2 -5 -20 0.20 2.50 2 5 -20 2.30 4.30 2 -5 20 -1.40 3.10 -2 5 20 1.60 4.20 2 5 20 -4.50 3.20 2 -5 -20 4.30 3.80 -2 5 -20 3.40 4.10 -2 -5 20 2.30 4.30 -2 5 -20 0.20 2.70 -2 5 -20 5.00 3.50 2 -5 -20 0.60 3.60 -2 -5 20 -0.90 3.60 0 -6 -20 76.19 8.10 0 6 20 83.79 9.20 0 6 20 80.19 9.10 0 -6 20 100.69 9.90 0 -6 20 83.49 9.20 0 6 -20 80.59 9.10 0 -6 -20 86.49 8.80 1 6 -20 11.20 3.90 1 6 -20 15.20 5.20 1 -6 20 12.50 4.50 -1 6 20 15.50 5.10 1 -6 20 11.30 4.40 -1 -6 -20 13.50 4.00 -1 6 20 19.90 6.10 -1 6 -20 10.90 5.00 -1 -6 20 5.90 4.80 -1 -6 20 15.20 4.80 -1 6 -20 9.80 3.70 1 -6 -20 8.10 4.00 1 6 20 15.60 5.20 -1 -6 20 11.10 4.70 1 -6 -20 4.40 4.10 2 6 -20 7.40 4.20 -2 6 20 10.60 5.40 2 -6 20 8.10 4.90 -2 6 20 8.00 4.90 -2 6 20 5.80 5.20 -2 -6 -20 8.90 3.50 2 -6 20 13.70 4.50 -2 6 -20 14.40 4.50 -2 -6 20 9.80 4.50 -2 6 -20 7.80 4.80 -2 -6 20 6.00 4.50 2 -6 -20 7.10 3.70 2 6 20 5.50 4.10 2 -6 -20 12.60 5.20 0 7 20 5.90 4.60 0 7 20 11.30 4.90 0 -7 -20 12.90 4.10 0 -7 -20 11.80 5.10 0 -7 20 9.50 4.50 0 -7 20 14.00 5.00 0 7 -20 14.60 4.30 0 7 -20 14.60 5.10 1 -7 20 16.20 5.30 -1 7 20 15.70 5.60 1 7 -20 18.50 5.30 -1 -7 -20 11.30 3.70 -1 7 20 24.40 6.60 1 -7 20 13.20 4.80 1 7 -20 11.00 4.00 -1 7 -20 5.00 3.50 1 -7 -20 14.50 4.50 -1 -7 20 5.80 4.60 1 7 20 10.90 4.80 -1 7 -20 8.40 4.90 -1 -7 20 14.80 4.90 1 -7 -20 11.00 4.90 -1 -7 20 11.50 4.80 2 7 -20 21.50 5.40 -2 7 20 15.50 6.60 -2 7 20 19.80 6.30 -2 -7 -20 16.10 4.30 2 -7 20 16.80 4.90 2 -7 20 15.60 5.00 -2 7 20 20.10 6.60 -2 7 -20 19.10 5.50 2 7 20 10.90 4.80 2 -7 -20 18.40 5.50 2 -7 -20 25.30 5.50 -2 -7 20 21.40 5.70 -2 7 -20 22.00 5.10 -2 -7 20 18.60 5.30 0 8 20 202.38 13.50 0 8 20 203.18 13.40 0 -8 20 213.28 12.80 0 8 -20 209.08 13.10 0 -8 20 192.28 12.40 0 -8 -20 210.48 12.20 0 -8 -20 219.08 13.30 0 8 -20 210.18 12.20 1 8 -20 53.59 7.60 -1 8 20 49.80 8.50 1 -8 20 41.40 6.80 -1 -8 -20 39.00 5.90 1 8 -20 52.49 7.10 -1 8 20 52.49 8.40 1 -8 20 48.60 7.40 1 -8 -20 44.00 6.80 -1 8 -20 53.19 7.30 -1 8 -20 49.30 7.70 -1 -8 20 48.80 7.30 -1 -8 20 37.40 7.30 1 -8 -20 43.50 7.20 -1 -8 20 52.69 7.60 1 8 20 41.60 7.20 -2 8 20 38.80 7.90 -2 8 20 23.10 7.20 2 8 -20 31.50 6.40 2 -8 20 37.90 6.60 2 -8 -20 37.30 7.00 2 8 20 39.40 6.70 -2 -8 20 29.70 6.00 -2 8 -20 39.80 7.30 0 -9 20 7.00 4.90 0 -9 -20 11.40 4.10 0 -9 -20 9.90 4.80 0 9 -20 9.60 4.20 0 9 20 9.70 5.20 0 9 20 8.20 5.60 0 -9 20 4.40 4.20 0 9 -20 8.90 4.60 1 -9 20 48.50 7.30 -1 9 20 44.80 8.30 1 -9 20 53.89 8.00 -1 -9 -20 56.79 7.30 1 9 -20 62.19 7.80 1 9 -20 48.10 7.30 -1 9 20 50.39 9.00 -1 -9 20 50.59 7.70 -1 -9 20 49.80 7.30 -1 9 -20 58.39 8.20 1 -9 -20 57.29 8.30 1 -9 -20 65.59 8.40 -1 9 -20 58.29 7.90 1 9 20 56.89 8.60 0 -10 20 160.68 11.60 0 -10 20 154.28 11.40 0 10 -20 159.98 11.10 0 -10 -20 146.89 18.20 0 10 20 148.89 12.40 0 10 20 153.78 12.50 0 -10 -20 171.28 11.30 0 10 -20 156.58 11.80 0 0 21 3.30 3.60 0 0 -21 0.50 3.50 0 0 -21 -2.70 2.40 0 0 21 0.70 3.70 -1 0 -21 -0.60 3.60 1 0 -21 0.40 3.50 -1 0 21 -0.80 3.30 -1 0 21 3.80 4.20 -1 0 -21 2.80 2.80 1 0 21 0.00 3.70 1 0 -21 0.20 2.70 1 0 21 1.80 3.50 2 0 -21 77.29 8.90 -2 0 21 86.69 9.80 2 0 21 100.59 9.90 -2 0 -21 75.59 8.00 2 0 -21 92.69 9.40 -2 0 21 65.59 9.40 -2 0 21 99.09 10.20 0 -1 -21 2.20 2.80 0 -1 -21 5.70 4.30 0 1 -21 3.00 2.70 0 -1 21 2.90 3.90 0 -1 21 1.80 3.80 0 1 21 5.20 4.10 0 1 21 -3.10 3.10 0 1 -21 4.40 3.80 1 -1 21 24.30 5.50 1 -1 21 28.10 5.90 -1 1 21 31.70 6.40 1 1 -21 32.30 5.80 1 1 -21 32.20 6.30 -1 1 21 42.00 6.90 -1 -1 -21 34.60 6.40 -1 -1 -21 33.40 5.60 1 -1 -21 35.30 6.30 -1 -1 21 32.60 6.40 1 -1 -21 37.60 5.90 1 1 21 40.00 6.60 1 1 21 41.90 6.90 -1 1 -21 40.50 7.00 -1 -1 21 33.10 6.70 -1 1 -21 32.00 5.50 2 1 -21 11.20 3.80 -2 1 21 13.30 5.40 2 -1 21 8.30 4.00 -2 1 21 14.70 6.20 2 1 -21 13.50 5.00 -2 -1 -21 18.60 4.60 -2 1 21 3.00 4.40 -2 -1 21 7.30 4.50 2 -1 -21 18.00 4.90 2 1 21 10.40 4.40 2 -1 -21 11.70 4.80 -2 -1 21 13.80 4.80 -2 -1 21 12.70 5.80 -2 1 -21 12.20 3.90 0 -2 -21 4.90 4.30 0 -2 -21 4.00 3.30 0 2 21 5.30 4.00 0 2 -21 7.30 3.60 0 2 -21 5.30 4.20 0 -2 21 2.30 4.00 0 2 21 6.30 4.20 0 -2 21 5.80 3.90 -1 2 21 13.00 5.40 1 -2 21 21.80 5.10 -1 -2 -21 19.80 5.50 -1 2 21 10.60 5.20 1 2 -21 15.60 4.20 1 2 -21 11.00 4.60 1 -2 21 16.20 4.60 -1 -2 -21 17.90 4.30 1 2 21 21.80 5.70 1 -2 -21 15.20 5.10 -1 -2 21 13.30 4.90 -1 2 -21 20.40 5.50 1 -2 -21 15.70 4.40 1 2 21 20.00 5.50 -1 -2 21 19.30 5.10 -1 2 -21 19.90 4.70 2 2 -21 9.60 3.90 -2 -2 -21 11.20 3.90 2 -2 21 13.60 4.70 2 2 -21 7.90 4.50 -2 2 21 9.30 5.10 -2 2 21 8.10 4.90 -2 2 21 17.60 6.70 2 -2 -21 7.00 4.30 -2 -2 21 10.00 4.90 -2 -2 21 -1.20 4.20 -2 -2 21 12.60 5.20 2 2 21 7.10 4.00 2 -2 -21 11.60 4.10 0 3 21 90.29 9.50 0 -3 -21 97.29 8.30 0 3 -21 86.29 8.90 0 -3 21 94.79 9.80 0 -3 -21 84.89 9.00 0 3 -21 85.89 9.40 0 3 21 120.69 10.20 0 -3 21 97.09 9.80 -1 3 21 17.30 5.50 -1 -3 -21 15.90 4.10 1 -3 21 15.40 5.20 1 3 -21 9.00 4.50 1 -3 21 10.50 4.20 -1 -3 -21 10.50 4.50 1 3 -21 14.80 4.10 -1 3 21 12.30 5.10 1 3 21 6.40 4.00 1 -3 -21 10.50 3.80 -1 -3 21 14.70 5.20 -1 3 -21 16.70 4.70 1 -3 -21 10.20 4.60 -1 3 -21 16.50 5.10 1 3 21 13.40 4.90 -1 -3 21 17.00 5.10 -2 3 21 -2.50 4.00 2 3 -21 7.40 4.50 2 3 -21 2.50 3.40 -2 3 21 4.20 4.80 -2 -3 -21 -0.10 2.50 2 -3 21 -0.20 3.30 -2 3 21 5.40 5.10 -2 -3 21 0.20 4.20 2 3 21 1.70 3.60 -2 -3 21 -0.10 4.40 2 -3 -21 5.70 4.30 -2 3 -21 2.30 2.80 -2 -3 21 -0.40 3.90 2 -3 -21 4.90 3.60 0 -4 -21 68.19 7.70 0 4 -21 73.69 8.30 0 4 21 92.89 10.10 0 -4 21 56.19 7.40 0 -4 21 77.89 9.20 0 -4 -21 59.89 7.70 0 4 -21 77.59 8.70 0 4 21 77.29 8.90 1 4 -21 19.20 5.00 1 4 -21 26.30 6.00 1 -4 21 23.80 5.40 -1 -4 -21 33.40 5.90 1 -4 21 11.60 4.80 -1 4 21 15.80 5.80 -1 4 21 16.90 5.70 1 -4 -21 28.20 6.50 -1 -4 21 22.30 6.00 1 4 21 20.00 5.40 -1 -4 21 28.70 6.00 -1 4 -21 19.00 5.80 1 -4 -21 25.60 5.50 1 4 21 25.70 6.20 -2 4 21 65.09 9.10 -2 4 21 52.69 8.50 -2 4 21 61.19 9.60 2 4 -21 66.09 8.00 2 -4 21 54.49 7.50 2 4 -21 60.09 8.10 -2 -4 -21 46.70 6.40 2 4 21 53.99 7.80 2 -4 -21 53.79 7.20 -2 -4 21 39.00 7.70 -2 -4 21 52.59 7.70 2 -4 -21 58.89 8.30 -2 4 -21 52.09 7.00 0 -5 21 8.10 4.60 0 5 21 11.90 5.10 0 -5 21 8.80 4.30 0 -5 -21 7.10 4.30 0 5 -21 5.10 4.40 0 -5 -21 7.40 3.80 0 5 21 10.40 5.00 0 5 -21 7.30 3.50 1 5 -21 32.80 6.00 -1 5 21 22.00 6.10 -1 5 21 33.90 6.80 -1 -5 -21 25.90 5.00 1 -5 21 29.40 6.00 1 5 -21 34.50 6.50 1 -5 21 24.00 5.50 1 -5 -21 34.30 6.50 1 -5 -21 24.00 5.10 -1 -5 21 20.80 6.70 -1 5 -21 26.60 5.90 -1 5 -21 34.40 5.90 -1 -5 21 27.00 6.10 1 5 21 29.60 6.00 -1 -5 21 42.00 6.80 2 5 -21 26.30 5.90 -2 5 21 24.40 6.70 -2 5 21 19.70 7.00 2 -5 21 24.10 5.50 -2 5 21 24.30 6.90 -2 -5 21 13.80 5.70 2 -5 -21 39.50 7.40 -2 -5 21 22.90 5.80 2 5 21 22.10 5.40 -2 5 -21 21.70 4.80 -2 5 -21 18.40 4.80 0 -6 -21 8.80 3.80 0 -6 -21 11.80 4.80 0 6 -21 13.80 5.10 0 6 21 8.40 5.00 0 6 -21 11.50 4.30 0 -6 21 13.30 5.00 0 -6 21 6.90 4.70 0 6 21 11.20 5.00 -1 6 21 5.80 5.20 -1 6 21 4.00 4.90 -1 -6 -21 8.90 3.40 1 -6 21 12.60 4.90 1 -6 21 10.20 4.80 1 6 -21 3.20 3.80 1 6 21 1.60 4.10 -1 -6 21 5.70 4.30 -1 -6 21 -3.30 3.60 1 -6 -21 5.80 3.50 -1 6 -21 4.50 3.90 -1 6 -21 7.40 4.60 1 -6 -21 0.50 4.00 -1 -6 21 7.80 5.60 0 7 -21 187.88 12.80 0 -7 -21 198.88 12.10 0 7 21 186.18 13.10 0 7 21 183.38 13.20 0 -7 -21 224.18 13.50 0 -7 21 194.38 12.50 0 7 -21 201.18 12.20 0 -7 21 195.18 12.60 1 -7 21 29.70 6.30 -1 -7 -21 19.30 4.50 -1 7 21 26.50 6.50 1 -7 21 25.90 5.90 1 7 -21 28.60 5.70 -1 7 21 29.30 7.00 1 7 -21 24.40 6.00 -1 7 -21 18.30 4.90 -1 -7 21 33.50 6.20 -1 -7 21 30.80 6.70 -1 7 -21 30.60 6.50 1 -7 -21 29.40 5.70 1 7 21 25.10 6.00 -1 -7 21 26.10 5.90 1 -7 -21 24.50 6.40 0 -8 21 96.79 9.80 0 -8 -21 104.29 9.10 0 8 21 80.99 9.90 0 8 21 95.29 11.10 0 8 -21 95.69 10.00 0 -8 21 91.19 9.70 0 -8 -21 96.99 10.20 0 8 -21 96.09 8.50 0 0 22 299.27 15.80 0 0 -22 327.37 16.40 0 0 -22 314.47 15.00 0 0 22 291.67 15.40 1 0 -22 26.30 5.30 -1 0 -22 33.50 6.40 1 0 22 26.60 5.80 -1 0 22 33.20 6.50 1 0 -22 34.80 6.50 1 0 22 22.90 5.90 -1 0 -22 27.40 5.30 -1 0 22 28.20 6.30 0 -1 -22 2.80 3.40 0 -1 22 5.80 4.60 0 1 22 13.80 5.10 0 -1 22 5.00 4.30 0 1 22 6.00 4.20 0 1 -22 9.10 4.00 0 -1 -22 8.00 4.60 0 1 -22 11.80 5.30 -1 -1 -22 79.09 9.40 -1 1 22 66.69 8.70 1 1 -22 61.09 8.30 -1 -1 -22 68.59 7.80 1 -1 22 63.59 8.40 -1 1 22 61.69 8.50 1 -1 22 64.79 8.30 1 1 -22 60.69 7.60 -1 -1 22 59.39 8.10 1 1 22 57.89 8.10 -1 1 -22 70.39 8.90 -1 -1 22 61.89 8.00 1 -1 -22 57.69 8.00 -1 1 -22 65.79 7.80 1 -1 -22 58.59 7.50 1 1 22 65.29 7.90 0 2 -22 -1.30 3.70 0 2 22 5.60 4.80 0 -2 -22 3.40 3.60 0 -2 22 6.30 4.70 0 2 -22 5.10 3.60 0 -2 22 0.20 3.70 0 2 22 -1.00 4.20 0 -2 -22 2.70 4.30 1 2 -22 35.80 6.90 -1 -2 -22 37.10 9.20 -1 2 22 43.00 7.50 1 -2 22 33.30 6.70 -1 2 22 31.70 6.60 1 -2 22 28.90 6.20 -1 -2 -22 30.40 5.90 1 2 -22 30.80 5.90 1 -2 -22 32.90 6.70 -1 -2 22 24.90 6.10 -1 -2 22 37.00 7.10 1 2 22 26.50 5.90 1 2 22 35.60 6.80 1 -2 -22 32.90 6.00 -1 2 -22 22.20 5.00 -1 2 -22 34.70 6.90 0 -3 22 4.40 4.50 0 3 22 -0.10 3.90 0 3 22 0.40 4.50 0 -3 -22 -0.10 3.80 0 -3 -22 -0.60 2.60 0 3 -22 5.70 3.50 0 3 -22 -1.30 3.70 0 -3 22 2.60 3.70 1 -3 22 53.79 7.90 1 3 -22 41.70 7.00 -1 3 22 56.39 8.70 -1 -3 -22 49.10 6.70 1 -3 22 50.69 7.50 1 3 -22 54.49 7.20 -1 3 22 69.49 9.50 -1 3 -22 49.20 7.70 1 -3 -22 49.00 7.30 1 -3 -22 61.09 8.80 -1 -3 22 51.59 7.60 -1 -3 22 58.59 8.40 -1 3 -22 50.79 7.00 1 3 22 54.59 8.00 1 3 22 55.09 8.10 0 -4 22 116.29 11.30 0 -4 -22 86.59 9.10 0 4 -22 101.59 10.70 0 4 -22 95.59 8.30 0 4 22 111.09 11.50 0 -4 -22 100.49 10.60 0 -4 22 84.29 9.30 0 4 22 93.49 10.40 1 -4 22 29.90 6.00 -1 -4 -22 32.00 5.90 1 4 -22 32.30 6.90 -1 4 22 28.10 7.00 1 -4 22 30.40 6.10 1 4 -22 35.90 6.20 -1 4 22 39.20 7.20 -1 -4 22 19.20 7.00 1 -4 -22 28.80 6.30 1 -4 -22 21.00 5.00 -1 4 -22 25.30 6.20 1 4 22 37.50 7.00 -1 -4 22 25.70 6.40 -1 -4 22 31.10 6.80 0 5 -22 11.50 5.50 0 5 22 11.40 5.30 0 5 22 18.60 5.70 0 -5 -22 9.10 5.20 0 -5 -22 7.00 3.70 0 -5 22 4.00 4.20 0 -5 22 10.70 5.30 -1 -5 22 27.80 7.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 22218 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1 S 0.65312(9) 0.60476(3) 0.50392(2) 0.02013(11) Uani 1 1 d . O1 O 1.0272(2) 0.67889(9) 0.76314(7) 0.0213(3) Uani 1 1 d . N1 N 0.6032(3) 0.66535(9) 0.72264(9) 0.0159(3) Uani 1 1 d . C1 C 0.5368(3) 0.59791(11) 0.59788(9) 0.0164(3) Uani 1 1 d . C2 C 0.6632(3) 0.65490(10) 0.64319(9) 0.0156(3) Uani 1 1 d . C3 C 0.8529(4) 0.70254(11) 0.60268(10) 0.0181(3) Uani 1 1 d . H3 H 0.956220 0.744222 0.626035 0.022 Uiso 1 1 calc R C4 C 0.8696(4) 0.68167(11) 0.52657(10) 0.0207(4) Uani 1 1 d . H4 H 0.986496 0.706568 0.490578 0.025 Uiso 1 1 calc R C5 C 0.3259(4) 0.53729(11) 0.62046(10) 0.0182(3) Uani 1 1 d . H5 H 0.167073 0.569061 0.637182 0.022 Uiso 1 1 calc R C6 C 0.2430(4) 0.48427(12) 0.55153(10) 0.0228(4) Uani 1 1 d . H6A H 0.182143 0.519373 0.509207 0.034 Uiso 1 1 calc GR H6B H 0.099336 0.447714 0.567273 0.034 Uiso 1 1 calc GR H6C H 0.394405 0.451825 0.534028 0.034 Uiso 1 1 calc GR C7 C 0.4070(3) 0.48271(11) 0.68798(10) 0.0180(4) Uani 1 1 d . C8 C 0.6185(4) 0.42915(13) 0.68140(12) 0.0281(4) Uani 1 1 d . H8 H 0.723718 0.429957 0.635871 0.034 Uiso 1 1 calc R C9 C 0.6792(4) 0.37440(13) 0.74013(13) 0.0319(5) Uani 1 1 d . H9 H 0.823610 0.337829 0.734353 0.038 Uiso 1 1 calc R C10 C 0.5294(4) 0.37317(12) 0.80690(12) 0.0288(5) Uani 1 1 d . H10 H 0.570118 0.335827 0.847230 0.035 Uiso 1 1 calc R C11 C 0.3208(5) 0.42646(13) 0.81459(11) 0.0336(5) Uani 1 1 d . H11 H 0.217986 0.426018 0.860584 0.040 Uiso 1 1 calc R C12 C 0.2589(4) 0.48120(12) 0.75536(11) 0.0263(4) Uani 1 1 d . H12 H 0.114250 0.517650 0.761333 0.032 Uiso 1 1 calc R C13 C 0.7893(3) 0.67717(11) 0.77770(10) 0.0161(3) Uani 1 1 d . C14 C 0.6864(3) 0.68539(12) 0.85975(10) 0.0210(4) Uani 1 1 d . H14 H 0.490163 0.692735 0.858315 0.025 Uiso 1 1 calc R C15 C 0.7516(5) 0.60675(16) 0.90324(13) 0.0414(6) Uani 1 1 d . H15A H 0.676463 0.560072 0.875433 0.062 Uiso 1 1 calc GR H15B H 0.676222 0.609270 0.955423 0.062 Uiso 1 1 calc GR H15C H 0.943958 0.600470 0.906763 0.062 Uiso 1 1 calc GR C16 C 0.8118(5) 0.75944(15) 0.89862(13) 0.0361(5) Uani 1 1 d . H16A H 1.004619 0.753541 0.898391 0.054 Uiso 1 1 calc GR H16B H 0.748871 0.763395 0.952124 0.054 Uiso 1 1 calc GR H16C H 0.762378 0.808988 0.870331 0.054 Uiso 1 1 calc GR H1 H 0.455(6) 0.6649(15) 0.7361(14) 0.035(7) 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 S1 0.0233(2) 0.0222(2) 0.01486(18) 0.00153(17) 0.00140(17) -0.00131(18) O1 0.0120(6) 0.0290(7) 0.0228(7) -0.0020(6) 0.0000(5) -0.0001(5) N1 0.0107(7) 0.0205(8) 0.0165(7) 0.0001(6) 0.0026(5) 0.0002(6) C1 0.0158(7) 0.0180(8) 0.0153(7) 0.0027(7) 0.0012(6) 0.0024(7) C2 0.0137(7) 0.0164(8) 0.0167(7) 0.0015(6) -0.0001(7) 0.0035(7) C3 0.0169(8) 0.0172(8) 0.0202(8) 0.0034(6) -0.0002(7) 0.0004(7) C4 0.0200(8) 0.0210(8) 0.0210(8) 0.0060(7) 0.0021(7) -0.0014(8) C5 0.0166(8) 0.0190(8) 0.0189(8) 0.0009(6) 0.0007(7) 0.0004(7) C6 0.0231(9) 0.0244(9) 0.0207(9) -0.0001(7) -0.0034(7) -0.0030(7) C7 0.0190(9) 0.0176(8) 0.0173(8) 0.0003(7) -0.0009(6) -0.0047(7) C8 0.0213(9) 0.0360(11) 0.0269(10) 0.0087(8) 0.0060(8) 0.0052(8) C9 0.0279(10) 0.0323(11) 0.0356(11) 0.0093(9) -0.0028(9) 0.0040(9) C10 0.0412(12) 0.0228(10) 0.0224(9) 0.0071(8) -0.0097(8) -0.0078(9) C11 0.0472(13) 0.0350(11) 0.0185(9) 0.0020(8) 0.0086(9) -0.0049(10) C12 0.0326(10) 0.0245(11) 0.0217(9) -0.0016(8) 0.0065(8) 0.0008(8) C13 0.0156(8) 0.0142(8) 0.0184(8) 0.0008(7) -0.0003(6) 0.0013(6) C14 0.0154(8) 0.0297(10) 0.0180(8) -0.0007(7) 0.0018(6) -0.0009(8) C15 0.0540(14) 0.0433(13) 0.0270(10) 0.0134(10) 0.0063(10) -0.0032(12) C16 0.0408(13) 0.0424(12) 0.0252(10) -0.0136(9) 0.0040(9) -0.0060(11) 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 C4 S1 C1 92.89(9) C13 N1 C2 123.40(15) C2 C1 S1 109.40(13) C2 C1 C5 128.89(15) C5 C1 S1 121.70(13) N1 C2 C3 123.75(15) C1 C2 N1 122.30(16) C1 C2 C3 113.94(15) C4 C3 C2 112.33(16) C3 C4 S1 111.43(14) C1 C5 C6 111.44(14) C1 C5 C7 113.19(14) C7 C5 C6 109.61(15) C8 C7 C5 120.98(16) C12 C7 C5 120.55(17) C12 C7 C8 118.31(17) C7 C8 C9 121.24(18) C10 C9 C8 119.95(19) C11 C10 C9 119.47(18) C10 C11 C12 120.58(19) C7 C12 C11 120.44(19) O1 C13 N1 122.69(16) O1 C13 C14 121.67(15) N1 C13 C14 115.61(15) C13 C14 C15 108.13(16) C13 C14 C16 109.88(16) C16 C14 C15 111.39(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C1 1.7309(17) S1 C4 1.7147(19) O1 C13 1.230(2) N1 C2 1.417(2) N1 C13 1.352(2) C1 C2 1.376(2) C1 C5 1.509(2) C2 C3 1.421(2) C3 C4 1.362(3) C5 C6 1.533(2) C5 C7 1.526(2) C7 C8 1.388(3) C7 C12 1.385(3) C8 C9 1.389(3) C9 C10 1.380(3) C10 C11 1.376(3) C11 C12 1.397(3) C13 C14 1.516(2) C14 C15 1.528(3) C14 C16 1.525(3)