#------------------------------------------------------------------------------ #$Date: 2020-09-16 03:04:15 +0300 (Wed, 16 Sep 2020) $ #$Revision: 256436 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/90/1559091.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_1559091 loop_ _publ_author_name 'Lv, Mengya' 'Zhang, Yanhao' 'Fan, Jiayi' 'Yang, Yanyun' 'Chen, Sheng' 'Liang, Gaolin' 'Zhang, Shusheng' _publ_section_title ; A near-infrared fluorescent probe for ratiometric sensing of SO2 in cells and zebrafish ; _journal_name_full 'The Analyst' _journal_paper_doi 10.1039/D0AN01468K _journal_year 2020 _chemical_formula_moiety 'C28 H27 N O4 S, 2(C H2 Cl2)' _chemical_formula_sum 'C30 H31 Cl4 N O4 S' _chemical_formula_weight 643.42 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2018-06-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-11 deposited with the CCDC. 2020-09-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.2798(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.68126(19) _cell_length_b 22.6995(5) _cell_length_c 17.9400(3) _cell_measurement_reflns_used 4273 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 70.6700 _cell_measurement_theta_min 3.8930 _cell_volume 3114.76(12) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _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 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -46.00 -2.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - -33.5000 37.0000 -30.0000 88 #__ type_ start__ end____ width___ exp.time_ 2 omega -27.00 33.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - -33.5000 77.0000 -180.0000 120 #__ type_ start__ end____ width___ exp.time_ 3 omega 6.00 36.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - -33.5000 37.0000 -150.0000 60 #__ type_ start__ end____ width___ exp.time_ 4 omega 15.00 100.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 37.0000 90.0000 170 #__ type_ start__ end____ width___ exp.time_ 5 omega 60.00 108.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 178.0000 -60.0000 96 #__ type_ start__ end____ width___ exp.time_ 6 omega 35.00 69.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 -99.0000 90.0000 68 #__ type_ start__ end____ width___ exp.time_ 7 omega 70.00 104.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 77.0000 0.0000 68 #__ type_ start__ end____ width___ exp.time_ 8 omega 43.00 77.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 -99.0000 -60.0000 68 #__ type_ start__ end____ width___ exp.time_ 9 omega 31.00 63.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 57.0000 120.0000 64 #__ type_ start__ end____ width___ exp.time_ 10 omega -3.00 23.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 -99.0000 90.0000 52 #__ type_ start__ end____ width___ exp.time_ 11 omega 25.00 54.00 0.5000 1.7500 omega____ theta____ kappa____ phi______ frames - 36.4734 77.0000 0.0000 58 #__ type_ start__ end____ width___ exp.time_ 12 omega 89.00 149.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 61.0000 90.0000 120 #__ type_ start__ end____ width___ exp.time_ 13 omega 38.00 109.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 150.0000 142 #__ type_ start__ end____ width___ exp.time_ 14 omega 55.00 98.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 120.0000 86 #__ type_ start__ end____ width___ exp.time_ 15 omega 137.00 163.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -60.0000 52 #__ type_ start__ end____ width___ exp.time_ 16 omega 43.00 108.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 -90.0000 130 #__ type_ start__ end____ width___ exp.time_ 17 omega 61.00 89.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -30.0000 56 #__ type_ start__ end____ width___ exp.time_ 18 omega 48.00 86.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 150.0000 76 #__ type_ start__ end____ width___ exp.time_ 19 omega 44.00 78.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -90.0000 68 #__ type_ start__ end____ width___ exp.time_ 20 omega 44.00 90.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -60.0000 92 #__ type_ start__ end____ width___ exp.time_ 21 omega 71.00 99.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 90.0000 56 #__ type_ start__ end____ width___ exp.time_ 22 omega 48.00 87.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 -30.0000 -180.0000 78 #__ type_ start__ end____ width___ exp.time_ 23 omega 112.00 158.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 111.0000 -120.0000 92 #__ type_ start__ end____ width___ exp.time_ 24 omega 80.00 134.00 0.5000 17.5000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -60.0000 108 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0232088000 _diffrn_orient_matrix_UB_12 0.0672793000 _diffrn_orient_matrix_UB_13 0.0065989000 _diffrn_orient_matrix_UB_21 0.1803025000 _diffrn_orient_matrix_UB_22 -0.0050830000 _diffrn_orient_matrix_UB_23 -0.0306378000 _diffrn_orient_matrix_UB_31 -0.0868396000 _diffrn_orient_matrix_UB_32 0.0074262000 _diffrn_orient_matrix_UB_33 -0.0803069000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 13416 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.077 _diffrn_reflns_theta_max 67.077 _diffrn_reflns_theta_min 3.895 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.371 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.44521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.372 _exptl_crystal_description prism _exptl_crystal_F_000 1336 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _refine_diff_density_max 0.631 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 5563 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0683 _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^)+(0.1170P)^2^+1.7021P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1970 _refine_ls_wR_factor_ref 0.2148 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4269 _reflns_number_total 5563 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; 201806301.res created by SHELXL-2014/7 TITL 201806301 in P21/c #14 REM reset to P21/c #14 CELL 1.54184 7.68126 22.699495 17.939981 90 95.2798 90 ZERR 4 0.000186 0.000456 0.000323 0 0.0019 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O S UNIT 120 124 16 4 16 4 DFIX 1.43 O1A C9 DFIX 1.43 O1 C9 DFIX 1.43 C13A O1A DFIX 1.43 C13 O1 EADP C13 C13A EADP O1 O1A L.S. 4 PLAN 20 SIZE 0.13 0.14 0.16 MPLA C1 C2 C3 C4 C5 C6 C7 C8 C9 C10 MPLA C16 C17 C18 C19 C20 C21 C22 C23 N1 BOND $h conf fmap 2 acta REM REM REM WGHT 0.117000 1.702100 FVAR 1.94732 0.73439 C1 1 0.789320 0.591857 0.729197 11.00000 0.06569 0.05348 = 0.11055 0.00920 -0.00085 0.00253 AFIX 43 H1 2 0.796162 0.626036 0.701032 11.00000 -1.20000 AFIX 0 C2 1 0.757246 0.596025 0.801852 11.00000 0.06347 0.05887 = 0.12387 -0.01906 0.00759 0.00671 AFIX 43 H2 2 0.740458 0.632720 0.823106 11.00000 -1.20000 AFIX 0 C3 1 0.749390 0.544614 0.845128 11.00000 0.05924 0.07333 = 0.08462 -0.01694 0.01056 0.00488 AFIX 43 H3 2 0.730296 0.547738 0.895419 11.00000 -1.20000 AFIX 0 C4 1 0.769226 0.490360 0.814744 11.00000 0.05836 0.06271 = 0.06412 -0.00443 0.00838 -0.00090 AFIX 43 H4 2 0.762893 0.456955 0.844386 11.00000 -1.20000 AFIX 0 C5 1 0.799416 0.484278 0.738429 11.00000 0.04991 0.05304 = 0.05331 0.00457 0.00067 -0.00102 C6 1 0.812724 0.536462 0.695089 11.00000 0.05504 0.05462 = 0.07262 0.00958 -0.00636 -0.00426 C7 1 0.847455 0.530879 0.619132 11.00000 0.07835 0.06433 = 0.06580 0.02486 -0.00931 -0.01625 AFIX 43 H7 2 0.857807 0.564769 0.590747 11.00000 -1.20000 AFIX 0 C8 1 0.865883 0.477943 0.586901 11.00000 0.09227 0.07317 = 0.04699 0.01819 0.00199 -0.02235 AFIX 43 H8 2 0.890762 0.475647 0.537222 11.00000 -1.20000 AFIX 0 C9 1 0.847423 0.425996 0.628547 11.00000 0.06900 0.05957 = 0.04086 0.00872 0.00357 -0.01164 C10 1 0.816340 0.428533 0.703433 11.00000 0.06026 0.05131 = 0.04342 0.00703 0.00505 -0.00417 C11 1 0.802889 0.373362 0.741793 11.00000 0.09043 0.05135 = 0.03311 0.00312 0.01092 -0.00654 AFIX 43 H11 2 0.788803 0.373606 0.792728 11.00000 -1.20000 AFIX 0 C12 1 0.810034 0.321649 0.706382 11.00000 0.07167 0.05458 = 0.03776 0.00289 0.01205 -0.00466 PART 1 C13 1 0.812635 0.320786 0.621109 21.00000 0.10943 0.05468 = 0.03193 -0.00121 0.01202 -0.00942 AFIX 23 H13A 2 0.886348 0.288612 0.607324 21.00000 -1.20000 H13B 2 0.695172 0.313455 0.598331 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C13A 1 0.883500 0.324449 0.635636 -21.00000 0.10943 0.05468 = 0.03193 -0.00121 0.01202 -0.00942 AFIX 23 H13C 2 1.009715 0.327252 0.644510 -21.00000 -1.20000 H13D 2 0.856116 0.288282 0.608232 -21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.793171 0.268338 0.746446 11.00000 0.08473 0.05408 = 0.03522 0.00228 0.00910 -0.00344 AFIX 43 H14 2 0.780340 0.271849 0.797299 11.00000 -1.20000 AFIX 0 C15 1 0.793767 0.213059 0.718617 11.00000 0.07429 0.05414 = 0.03413 0.00143 0.00769 -0.00201 AFIX 43 H15 2 0.816509 0.208149 0.668968 11.00000 -1.20000 AFIX 0 C16 1 0.761789 0.162376 0.760731 11.00000 0.06091 0.05056 = 0.03356 -0.00133 0.00412 0.00180 C17 1 0.712411 0.158697 0.841289 11.00000 0.06953 0.04822 = 0.03199 0.00259 0.00802 0.00014 C18 1 0.684101 0.093614 0.848990 11.00000 0.06395 0.05340 = 0.03494 0.00290 0.00692 0.00007 C19 1 0.717949 0.065266 0.783440 11.00000 0.06038 0.04907 = 0.03613 0.00280 0.00408 -0.00031 C20 1 0.705863 0.004943 0.773762 11.00000 0.07697 0.04908 = 0.04511 -0.00239 0.00423 -0.00165 AFIX 43 H20 2 0.729430 -0.012945 0.729148 11.00000 -1.20000 AFIX 0 C21 1 0.656865 -0.027605 0.833846 11.00000 0.08246 0.04830 = 0.05645 0.00566 0.00396 -0.00707 AFIX 43 H21 2 0.646381 -0.068312 0.829636 11.00000 -1.20000 AFIX 0 C22 1 0.623328 -0.000211 0.900096 11.00000 0.08461 0.05994 = 0.05013 0.01623 0.01372 -0.00527 AFIX 43 H22 2 0.591401 -0.022964 0.939744 11.00000 -1.20000 AFIX 0 C23 1 0.636403 0.060490 0.908503 11.00000 0.08369 0.06130 = 0.03881 0.00657 0.01329 0.00118 AFIX 43 H23 2 0.613585 0.078457 0.953166 11.00000 -1.20000 AFIX 0 C24 1 0.867116 0.179107 0.896851 11.00000 0.08269 0.06331 = 0.04106 -0.00198 0.00048 -0.00101 AFIX 137 H24A 2 0.971549 0.158760 0.886191 11.00000 -1.50000 H24B 2 0.841839 0.170432 0.947108 11.00000 -1.50000 H24C 2 0.883781 0.220769 0.891667 11.00000 -1.50000 AFIX 0 C25 1 0.547213 0.194487 0.852917 11.00000 0.07899 0.05675 = 0.05748 -0.00030 0.01782 0.00302 AFIX 137 H25A 2 0.573799 0.235783 0.851779 11.00000 -1.50000 H25B 2 0.507146 0.184603 0.900485 11.00000 -1.50000 H25C 2 0.457513 0.185428 0.813752 11.00000 -1.50000 AFIX 0 C26 1 0.816144 0.093768 0.656947 11.00000 0.06237 0.04776 = 0.03814 -0.00096 0.01101 0.00015 AFIX 23 H26A 2 0.872196 0.055439 0.658564 11.00000 -1.20000 H26B 2 0.900365 0.122523 0.642648 11.00000 -1.20000 AFIX 0 C27 1 0.661525 0.092860 0.598625 11.00000 0.06158 0.06459 = 0.04075 -0.00037 0.01054 -0.00386 AFIX 23 H27A 2 0.586618 0.126334 0.606143 11.00000 -1.20000 H27B 2 0.594170 0.057256 0.604301 11.00000 -1.20000 AFIX 0 C28 1 0.720749 0.095180 0.519024 11.00000 0.07315 0.05866 = 0.03754 -0.00588 0.00795 -0.00360 AFIX 23 H28A 2 0.627855 0.079941 0.484010 11.00000 -1.20000 H28B 2 0.821924 0.069903 0.516699 11.00000 -1.20000 AFIX 0 N1 4 0.766131 0.108340 0.731853 11.00000 0.06493 0.04768 = 0.03310 0.00016 0.00753 0.00077 PART 1 O1 5 0.876094 0.375064 0.591850 21.00000 0.10366 0.06140 = 0.03940 0.00153 0.02327 -0.02336 PART 0 PART 2 O1A 5 0.820270 0.373110 0.591109 -21.00000 0.10366 0.06140 = 0.03940 0.00153 0.02327 -0.02336 PART 0 O2 5 0.927867 0.185408 0.539066 11.00000 0.09823 0.07574 = 0.05496 0.00397 0.00926 -0.02426 O3 5 0.623716 0.203110 0.502696 11.00000 0.10589 0.07662 = 0.08902 0.00847 0.02957 0.02781 O4 5 0.808702 0.163041 0.413715 11.00000 0.12409 0.07830 = 0.03723 0.00199 0.02227 0.00333 S1 6 0.775138 0.167918 0.491234 11.00000 0.07879 0.05534 = 0.03324 0.00014 0.01406 0.00557 C29 1 0.241570 0.358991 0.912320 11.00000 0.09841 0.10506 = 0.11031 0.01692 0.00962 -0.00357 AFIX 23 H29A 2 0.333221 0.341187 0.945750 11.00000 -1.20000 H29B 2 0.131877 0.340085 0.920805 11.00000 -1.20000 AFIX 0 CL1 3 0.285619 0.347892 0.820439 11.00000 0.23601 0.18264 = 0.12153 -0.01136 0.02945 0.07379 CL2 3 0.228515 0.434419 0.932067 11.00000 0.17924 0.09379 = 0.11752 0.00422 0.01064 0.00466 C30 1 0.709283 0.731008 0.440677 11.00000 0.08603 0.09609 = 0.11095 -0.03509 0.02573 -0.01226 AFIX 23 H30A 2 0.616697 0.752675 0.461801 11.00000 -1.20000 H30B 2 0.819728 0.749403 0.457853 11.00000 -1.20000 AFIX 0 CL3 3 0.709114 0.657589 0.472346 11.00000 0.13421 0.10750 = 0.09577 0.01407 0.02942 0.01575 CL4 3 0.678808 0.734606 0.343758 11.00000 0.18485 0.13491 = 0.10824 0.03733 -0.01903 -0.01787 HKLF 4 REM 201806301 in P21/c #14 REM R1 = 0.0683 for 4269 Fo > 4sig(Fo) and 0.0839 for all 5563 data REM 370 parameters refined using 4 restraints END WGHT 0.1170 1.6845 REM Highest difference peak 0.631, deepest hole -0.671, 1-sigma level 0.069 Q1 1 0.2266 0.3114 0.8535 11.00000 0.05 0.63 Q2 1 0.7424 0.6936 0.4911 11.00000 0.05 0.57 Q3 1 0.5904 0.6600 0.4411 11.00000 0.05 0.53 Q4 1 0.3950 0.3641 0.8499 11.00000 0.05 0.41 Q5 1 0.2358 0.4040 0.9618 11.00000 0.05 0.38 Q6 1 0.6677 0.7536 0.3793 11.00000 0.05 0.34 Q7 1 0.6452 0.6995 0.3416 11.00000 0.05 0.34 Q8 1 0.9220 0.1611 0.5197 11.00000 0.05 0.30 Q9 1 0.1270 0.4305 0.9003 11.00000 0.05 0.29 Q10 1 0.3699 0.3402 0.8794 11.00000 0.05 0.28 Q11 1 0.2071 0.3685 0.8196 11.00000 0.05 0.27 Q12 1 0.3317 0.4231 0.8991 11.00000 0.05 0.24 Q13 1 0.9870 0.3878 0.6032 11.00000 0.05 0.22 Q14 1 0.8004 0.7303 0.3557 11.00000 0.05 0.21 Q15 1 0.7171 0.7494 0.3142 11.00000 0.05 0.21 Q16 1 0.6236 0.1788 0.4723 11.00000 0.05 0.21 Q17 1 0.8221 0.1669 0.4339 11.00000 0.05 0.20 Q18 1 0.5244 0.1921 0.5176 11.00000 0.05 0.19 Q19 1 0.7359 0.1667 0.8029 11.00000 0.05 0.18 Q20 1 0.8601 0.4280 0.6763 11.00000 0.05 0.18 REM The information below was added by Olex2. REM REM R1 = 0.0683 for 4269 Fo > 4sig(Fo) and 0.0839 for all 13686 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.63, deepest hole -0.67 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0839 REM R1_gt = 0.0683 REM wR_ref = 0.2148 REM GOOF = 1.050 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 13686 REM Reflections_gt = 4269 REM Parameters = n/a REM Hole = -0.67 REM Peak = 0.63 REM Flack = n/a ; _cod_data_source_file d0an01468k2.cif _cod_data_source_block 201806301 _cod_original_cell_volume 3114.76(11) _cod_database_code 1559091 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C15H15O3N1S1 _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 0.600 _shelx_estimated_absorpt_t_min 0.541 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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. Restrained distances O1A-C9 1.43 with sigma of 0.02 O1-C9 1.43 with sigma of 0.02 C13A-O1A 1.43 with sigma of 0.02 C13-O1 1.43 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C13) = Uanis(C13A) Uanis(O1) = Uanis(O1A) 4. Others Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(O1A)=1-FVAR(1) Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(O1)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C13A(H13C,H13D), C26(H26A,H26B), C27(H27A,H27B), C28(H28A, H28B), C29(H29A,H29B), C30(H30A,H30B) 5.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C11(H11), C14(H14), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23) 5.c Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C25(H25A,H25B,H25C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 C1 C 0.7893(6) 0.59186(18) 0.7292(3) 0.0771(12) Uani 1 1 d . . . . . H1 H 0.7962 0.6260 0.7010 0.093 Uiso 1 1 calc R . . . . C2 C 0.7572(6) 0.59602(19) 0.8019(3) 0.0821(13) Uani 1 1 d . . . . . H2 H 0.7405 0.6327 0.8231 0.099 Uiso 1 1 calc R . . . . C3 C 0.7494(5) 0.54461(19) 0.8451(3) 0.0722(10) Uani 1 1 d . . . . . H3 H 0.7303 0.5477 0.8954 0.087 Uiso 1 1 calc R . . . . C4 C 0.7692(5) 0.49036(17) 0.8147(2) 0.0616(8) Uani 1 1 d . . . . . H4 H 0.7629 0.4570 0.8444 0.074 Uiso 1 1 calc R . . . . C5 C 0.7994(4) 0.48428(15) 0.73843(19) 0.0523(7) Uani 1 1 d . . . . . C6 C 0.8127(5) 0.53646(16) 0.6951(2) 0.0615(9) Uani 1 1 d . . . . . C7 C 0.8475(5) 0.53088(18) 0.6191(2) 0.0705(11) Uani 1 1 d . . . . . H7 H 0.8578 0.5648 0.5907 0.085 Uiso 1 1 calc R . . . . C8 C 0.8659(6) 0.47794(19) 0.5869(2) 0.0711(11) Uani 1 1 d . . . . . H8 H 0.8908 0.4756 0.5372 0.085 Uiso 1 1 calc R . . . . C9 C 0.8474(5) 0.42600(16) 0.62855(18) 0.0566(8) Uani 1 1 d D . . . . C10 C 0.8163(4) 0.42853(15) 0.70343(17) 0.0516(7) Uani 1 1 d . . . . . C11 C 0.8029(5) 0.37336(15) 0.74179(17) 0.0580(8) Uani 1 1 d . . . . . H11 H 0.7888 0.3736 0.7927 0.070 Uiso 1 1 calc R . . . . C12 C 0.8100(5) 0.32165(15) 0.70638(17) 0.0542(8) Uani 1 1 d . . . . . C13 C 0.8126(18) 0.3208(3) 0.6211(5) 0.065(2) Uani 0.73(2) 1 d D . P A 1 H13A H 0.8863 0.2886 0.6073 0.078 Uiso 0.73(2) 1 calc R . P A 1 H13B H 0.6952 0.3135 0.5983 0.078 Uiso 0.73(2) 1 calc R . P A 1 C13A C 0.884(5) 0.3244(11) 0.6356(13) 0.065(2) Uani 0.27(2) 1 d D . P A 2 H13C H 1.0097 0.3273 0.6445 0.078 Uiso 0.27(2) 1 calc R . P A 2 H13D H 0.8561 0.2883 0.6082 0.078 Uiso 0.27(2) 1 calc R . P A 2 C14 C 0.7932(5) 0.26834(15) 0.74645(17) 0.0578(8) Uani 1 1 d . . . . . H14 H 0.7803 0.2718 0.7973 0.069 Uiso 1 1 calc R . . . . C15 C 0.7938(5) 0.21306(15) 0.71862(17) 0.0540(8) Uani 1 1 d . . . . . H15 H 0.8165 0.2081 0.6690 0.065 Uiso 1 1 calc R . . . . C16 C 0.7618(4) 0.16238(14) 0.76073(16) 0.0484(7) Uani 1 1 d . . . . . C17 C 0.7124(5) 0.15870(14) 0.84129(16) 0.0497(7) Uani 1 1 d . . . . . C18 C 0.6841(4) 0.09361(15) 0.84899(16) 0.0506(7) Uani 1 1 d . . . . . C19 C 0.7179(4) 0.06527(14) 0.78344(16) 0.0485(7) Uani 1 1 d . . . . . C20 C 0.7059(5) 0.00494(15) 0.77376(19) 0.0571(8) Uani 1 1 d . . . . . H20 H 0.7294 -0.0129 0.7291 0.069 Uiso 1 1 calc R . . . . C21 C 0.6569(5) -0.02760(16) 0.8338(2) 0.0626(9) Uani 1 1 d . . . . . H21 H 0.6464 -0.0683 0.8296 0.075 Uiso 1 1 calc R . . . . C22 C 0.6233(5) -0.00021(17) 0.9001(2) 0.0644(9) Uani 1 1 d . . . . . H22 H 0.5914 -0.0230 0.9397 0.077 Uiso 1 1 calc R . . . . C23 C 0.6364(5) 0.06049(17) 0.90850(18) 0.0608(9) Uani 1 1 d . . . . . H23 H 0.6136 0.0785 0.9532 0.073 Uiso 1 1 calc R . . . . C24 C 0.8671(5) 0.17911(17) 0.89685(18) 0.0627(9) Uani 1 1 d . . . . . H24A H 0.9715 0.1588 0.8862 0.094 Uiso 1 1 calc GR . . . . H24B H 0.8418 0.1704 0.9471 0.094 Uiso 1 1 calc GR . . . . H24C H 0.8838 0.2208 0.8917 0.094 Uiso 1 1 calc GR . . . . C25 C 0.5472(5) 0.19449(17) 0.8529(2) 0.0637(9) Uani 1 1 d . . . . . H25A H 0.5738 0.2358 0.8518 0.096 Uiso 1 1 calc GR . . . . H25B H 0.5071 0.1846 0.9005 0.096 Uiso 1 1 calc GR . . . . H25C H 0.4575 0.1854 0.8138 0.096 Uiso 1 1 calc GR . . . . C26 C 0.8161(4) 0.09377(14) 0.65695(16) 0.0490(7) Uani 1 1 d . . . . . H26A H 0.8722 0.0554 0.6586 0.059 Uiso 1 1 calc R . . . . H26B H 0.9004 0.1225 0.6426 0.059 Uiso 1 1 calc R . . . . C27 C 0.6615(5) 0.09286(16) 0.59863(17) 0.0553(8) Uani 1 1 d . . . . . H27A H 0.5866 0.1263 0.6061 0.066 Uiso 1 1 calc R . . . . H27B H 0.5942 0.0573 0.6043 0.066 Uiso 1 1 calc R . . . . C28 C 0.7207(5) 0.09518(16) 0.51902(17) 0.0563(8) Uani 1 1 d . . . . . H28A H 0.6279 0.0799 0.4840 0.068 Uiso 1 1 calc R . . . . H28B H 0.8219 0.0699 0.5167 0.068 Uiso 1 1 calc R . . . . N1 N 0.7661(4) 0.10834(11) 0.73185(13) 0.0484(6) Uani 1 1 d . . . . . O1 O 0.8761(16) 0.3751(3) 0.5918(4) 0.067(2) Uani 0.73(2) 1 d D . P A 1 O1A O 0.820(3) 0.3731(8) 0.5911(13) 0.067(2) Uani 0.27(2) 1 d D . P A 2 O2 O 0.9279(4) 0.18541(13) 0.53907(15) 0.0762(8) Uani 1 1 d . . . . . O3 O 0.6237(5) 0.20311(14) 0.50270(19) 0.0892(9) Uani 1 1 d . . . . . O4 O 0.8087(5) 0.16304(13) 0.41372(14) 0.0790(8) Uani 1 1 d . . . . . S1 S 0.77514(12) 0.16792(4) 0.49123(4) 0.0552(3) Uani 1 1 d . . . . . C29 C 0.2416(8) 0.3590(3) 0.9123(4) 0.1046(17) Uani 1 1 d . . . . . H29A H 0.3332 0.3412 0.9457 0.126 Uiso 1 1 calc R . . . . H29B H 0.1319 0.3401 0.9208 0.126 Uiso 1 1 calc R . . . . Cl1 Cl 0.2856(4) 0.34789(13) 0.82044(14) 0.1793(11) Uani 1 1 d . . . . . Cl2 Cl 0.2285(3) 0.43442(8) 0.93207(11) 0.1304(6) Uani 1 1 d . . . . . C30 C 0.7093(7) 0.7310(2) 0.4407(3) 0.0967(16) Uani 1 1 d . . . . . H30A H 0.6167 0.7527 0.4618 0.116 Uiso 1 1 calc R . . . . H30B H 0.8197 0.7494 0.4579 0.116 Uiso 1 1 calc R . . . . Cl3 Cl 0.7091(2) 0.65759(7) 0.47235(9) 0.1113(5) Uani 1 1 d . . . . . Cl4 Cl 0.6788(3) 0.73461(10) 0.34376(11) 0.1447(8) Uani 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 C1 0.066(2) 0.053(2) 0.111(4) 0.009(2) -0.001(2) 0.0025(17) C2 0.063(2) 0.059(2) 0.124(4) -0.019(2) 0.008(2) 0.0067(18) C3 0.059(2) 0.073(2) 0.085(3) -0.017(2) 0.0106(18) 0.0049(18) C4 0.0584(19) 0.063(2) 0.064(2) -0.0044(16) 0.0084(16) -0.0009(16) C5 0.0499(16) 0.0530(17) 0.0533(17) 0.0046(14) 0.0007(13) -0.0010(13) C6 0.0550(18) 0.0546(19) 0.073(2) 0.0096(16) -0.0064(16) -0.0043(15) C7 0.078(2) 0.064(2) 0.066(2) 0.0249(18) -0.0093(18) -0.0163(19) C8 0.092(3) 0.073(2) 0.0470(18) 0.0182(17) 0.0020(18) -0.022(2) C9 0.069(2) 0.0596(19) 0.0409(16) 0.0087(14) 0.0036(14) -0.0116(16) C10 0.0603(18) 0.0513(17) 0.0434(16) 0.0070(13) 0.0050(13) -0.0042(14) C11 0.090(2) 0.0514(18) 0.0331(14) 0.0031(12) 0.0109(14) -0.0065(16) C12 0.072(2) 0.0546(18) 0.0378(15) 0.0029(13) 0.0120(14) -0.0047(15) C13 0.109(7) 0.055(2) 0.032(3) -0.001(2) 0.012(4) -0.009(4) C13A 0.109(7) 0.055(2) 0.032(3) -0.001(2) 0.012(4) -0.009(4) C14 0.085(2) 0.0541(18) 0.0352(14) 0.0023(13) 0.0091(14) -0.0034(16) C15 0.074(2) 0.0541(18) 0.0341(14) 0.0014(12) 0.0077(13) -0.0020(15) C16 0.0609(17) 0.0506(16) 0.0336(14) -0.0013(11) 0.0041(12) 0.0018(13) C17 0.0695(19) 0.0482(16) 0.0320(14) 0.0026(11) 0.0080(13) 0.0001(14) C18 0.0640(18) 0.0534(17) 0.0349(14) 0.0029(12) 0.0069(13) 0.0001(14) C19 0.0604(17) 0.0491(16) 0.0361(14) 0.0028(12) 0.0041(12) -0.0003(13) C20 0.077(2) 0.0491(17) 0.0451(17) -0.0024(13) 0.0042(15) -0.0017(15) C21 0.082(2) 0.0483(18) 0.0565(19) 0.0057(14) 0.0040(17) -0.0071(16) C22 0.085(2) 0.060(2) 0.0501(18) 0.0162(15) 0.0137(17) -0.0053(18) C23 0.084(2) 0.061(2) 0.0388(16) 0.0066(14) 0.0133(15) 0.0012(17) C24 0.083(2) 0.063(2) 0.0411(16) -0.0020(14) 0.0005(16) -0.0010(18) C25 0.079(2) 0.0568(19) 0.0575(19) -0.0003(15) 0.0178(17) 0.0030(17) C26 0.0624(18) 0.0478(16) 0.0381(15) -0.0010(12) 0.0110(13) 0.0002(13) C27 0.0616(19) 0.065(2) 0.0407(16) -0.0004(14) 0.0105(13) -0.0039(15) C28 0.073(2) 0.0587(19) 0.0375(15) -0.0059(13) 0.0079(14) -0.0036(16) N1 0.0649(15) 0.0477(14) 0.0331(12) 0.0002(10) 0.0075(10) 0.0008(11) O1 0.104(6) 0.0614(16) 0.0394(12) 0.0015(11) 0.023(3) -0.023(2) O1A 0.104(6) 0.0614(16) 0.0394(12) 0.0015(11) 0.023(3) -0.023(2) O2 0.098(2) 0.0757(17) 0.0550(14) 0.0040(12) 0.0093(13) -0.0243(15) O3 0.106(2) 0.0766(19) 0.089(2) 0.0085(16) 0.0296(18) 0.0278(17) O4 0.124(2) 0.0783(18) 0.0372(13) 0.0020(11) 0.0223(14) 0.0033(16) S1 0.0788(6) 0.0553(5) 0.0332(4) 0.0001(3) 0.0141(3) 0.0056(4) C29 0.098(4) 0.105(4) 0.110(4) 0.017(3) 0.010(3) -0.004(3) Cl1 0.236(3) 0.183(2) 0.1215(16) -0.0114(14) 0.0294(17) 0.074(2) Cl2 0.1792(18) 0.0938(10) 0.1175(12) 0.0042(8) 0.0106(11) 0.0047(10) C30 0.086(3) 0.096(4) 0.111(4) -0.035(3) 0.026(3) -0.012(3) Cl3 0.1342(12) 0.1075(10) 0.0958(9) 0.0141(7) 0.0294(8) 0.0157(9) Cl4 0.185(2) 0.1349(15) 0.1082(12) 0.0373(10) -0.0190(12) -0.0179(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 C2 C1 H1 119.3 . . ? C2 C1 C6 121.3(4) . . ? C6 C1 H1 119.3 . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.7(4) . . ? C3 C2 H2 120.2 . . ? C2 C3 H3 119.4 . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4 119.7 . . ? C3 C4 C5 120.6(4) . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C10 122.9(3) . . ? C10 C5 C6 118.9(3) . . ? C1 C6 C5 118.9(4) . . ? C1 C6 C7 122.5(4) . . ? C7 C6 C5 118.6(3) . . ? C6 C7 H7 119.0 . . ? C8 C7 C6 121.9(3) . . ? C8 C7 H7 119.0 . . ? C7 C8 H8 120.0 . . ? C7 C8 C9 119.9(4) . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.9(3) . . ? O1 C9 C8 115.2(4) . . ? O1 C9 C10 123.7(4) . . ? O1A C9 C8 119.1(11) . . ? O1A C9 C10 118.4(11) . . ? C5 C10 C11 123.4(3) . . ? C9 C10 C5 119.7(3) . . ? C9 C10 C11 117.0(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 C10 121.9(3) . . ? C12 C11 H11 119.0 . . ? C11 C12 C13 119.4(4) . . ? C11 C12 C13A 114.6(11) . . ? C11 C12 C14 119.9(3) . . ? C14 C12 C13 120.3(4) . . ? C14 C12 C13A 123.1(10) . . ? C12 C13 H13A 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? O1 C13 C12 112.9(8) . . ? O1 C13 H13A 109.0 . . ? O1 C13 H13B 109.0 . . ? C12 C13A H13C 109.0 . . ? C12 C13A H13D 109.0 . . ? H13C C13A H13D 107.8 . . ? O1A C13A C12 113(2) . . ? O1A C13A H13C 109.0 . . ? O1A C13A H13D 109.0 . . ? C12 C14 H14 116.5 . . ? C15 C14 C12 127.0(3) . . ? C15 C14 H14 116.5 . . ? C14 C15 H15 118.2 . . ? C14 C15 C16 123.6(3) . . ? C16 C15 H15 118.2 . . ? C15 C16 C17 128.4(3) . . ? N1 C16 C15 122.0(3) . . ? N1 C16 C17 109.5(3) . . ? C16 C17 C24 110.4(3) . . ? C16 C17 C25 112.3(3) . . ? C18 C17 C16 101.0(2) . . ? C18 C17 C24 110.1(3) . . ? C18 C17 C25 112.3(3) . . ? C25 C17 C24 110.4(3) . . ? C19 C18 C17 109.8(3) . . ? C23 C18 C17 131.1(3) . . ? C23 C18 C19 119.1(3) . . ? C18 C19 N1 108.3(3) . . ? C20 C19 C18 123.4(3) . . ? C20 C19 N1 128.3(3) . . ? C19 C20 H20 121.6 . . ? C19 C20 C21 116.7(3) . . ? C21 C20 H20 121.6 . . ? C20 C21 H21 119.6 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C21 C22 H22 119.3 . . ? C21 C22 C23 121.4(3) . . ? C23 C22 H22 119.3 . . ? C18 C23 C22 118.5(3) . . ? C18 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C17 C25 H25A 109.5 . . ? C17 C25 H25B 109.5 . . ? C17 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? H26A C26 H26B 107.8 . . ? C27 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? N1 C26 H26A 109.1 . . ? N1 C26 H26B 109.1 . . ? N1 C26 C27 112.5(3) . . ? C26 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C26 C27 C28 111.2(3) . . ? H27A C27 H27B 108.0 . . ? C28 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C27 C28 H28A 109.0 . . ? C27 C28 H28B 109.0 . . ? C27 C28 S1 112.8(2) . . ? H28A C28 H28B 107.8 . . ? S1 C28 H28A 109.0 . . ? S1 C28 H28B 109.0 . . ? C16 N1 C19 111.3(2) . . ? C16 N1 C26 125.5(3) . . ? C19 N1 C26 123.2(3) . . ? C9 O1 C13 118.4(6) . . ? C9 O1A C13A 112(2) . . ? O2 S1 C28 106.65(17) . . ? O3 S1 C28 105.08(19) . . ? O3 S1 O2 112.6(2) . . ? O3 S1 O4 113.5(2) . . ? O4 S1 C28 105.40(16) . . ? O4 S1 O2 112.75(19) . . ? H29A C29 H29B 108.1 . . ? Cl1 C29 H29A 109.5 . . ? Cl1 C29 H29B 109.5 . . ? Cl1 C29 Cl2 110.8(3) . . ? Cl2 C29 H29A 109.5 . . ? Cl2 C29 H29B 109.5 . . ? H30A C30 H30B 108.0 . . ? Cl3 C30 H30A 109.4 . . ? Cl3 C30 H30B 109.4 . . ? Cl4 C30 H30A 109.4 . . ? Cl4 C30 H30B 109.4 . . ? Cl4 C30 Cl3 111.3(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 C1 H1 0.9300 . ? C1 C2 1.352(7) . ? C1 C6 1.417(6) . ? C2 H2 0.9300 . ? C2 C3 1.406(7) . ? C3 H3 0.9300 . ? C3 C4 1.361(6) . ? C4 H4 0.9300 . ? C4 C5 1.416(5) . ? C5 C6 1.426(5) . ? C5 C10 1.424(5) . ? C6 C7 1.418(6) . ? C7 H7 0.9300 . ? C7 C8 1.347(6) . ? C8 H8 0.9300 . ? C8 C9 1.410(5) . ? C9 C10 1.387(5) . ? C9 O1 1.358(7) . ? C9 O1A 1.382(17) . ? C10 C11 1.437(5) . ? C11 H11 0.9300 . ? C11 C12 1.338(5) . ? C12 C13 1.532(9) . ? C12 C13A 1.44(3) . ? C12 C14 1.419(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 O1 1.442(9) . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C13A O1A 1.422(19) . ? C14 H14 0.9300 . ? C14 C15 1.351(5) . ? C15 H15 0.9300 . ? C15 C16 1.410(5) . ? C16 C17 1.530(4) . ? C16 N1 1.333(4) . ? C17 C18 1.501(5) . ? C17 C24 1.550(5) . ? C17 C25 1.537(5) . ? C18 C19 1.386(4) . ? C18 C23 1.383(5) . ? C19 C20 1.382(5) . ? C19 N1 1.419(4) . ? C20 H20 0.9300 . ? C20 C21 1.387(5) . ? C21 H21 0.9300 . ? C21 C22 1.386(5) . ? C22 H22 0.9300 . ? C22 C23 1.389(5) . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 C27 1.509(5) . ? C26 N1 1.469(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.539(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 S1 1.785(4) . ? O2 S1 1.444(3) . ? O3 S1 1.441(3) . ? O4 S1 1.442(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 Cl1 1.731(7) . ? C29 Cl2 1.753(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 Cl3 1.761(6) . ? C30 Cl4 1.735(6) . ? 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 C1 C2 C3 C4 -1.6(6) . . . . ? C1 C6 C7 C8 -178.6(4) . . . . ? C2 C1 C6 C5 0.9(6) . . . . ? C2 C1 C6 C7 -179.6(4) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C3 C4 C5 C6 1.5(5) . . . . ? C3 C4 C5 C10 -178.3(3) . . . . ? C4 C5 C6 C1 -2.2(5) . . . . ? C4 C5 C6 C7 178.4(3) . . . . ? C4 C5 C10 C9 -179.4(3) . . . . ? C4 C5 C10 C11 0.6(5) . . . . ? C5 C6 C7 C8 0.8(6) . . . . ? C5 C10 C11 C12 176.3(4) . . . . ? C6 C1 C2 C3 1.0(6) . . . . ? C6 C5 C10 C9 0.8(5) . . . . ? C6 C5 C10 C11 -179.2(3) . . . . ? C6 C7 C8 C9 1.2(6) . . . . ? C7 C8 C9 C10 -2.3(6) . . . . ? C7 C8 C9 O1 -177.2(7) . . . . ? C7 C8 C9 O1A 163.0(13) . . . . ? C8 C9 C10 C5 1.2(5) . . . . ? C8 C9 C10 C11 -178.8(4) . . . . ? C8 C9 O1 C13 -162.5(12) . . . . ? C8 C9 O1A C13A 153(2) . . . . ? C9 C10 C11 C12 -3.7(6) . . . . ? C10 C5 C6 C1 177.6(3) . . . . ? C10 C5 C6 C7 -1.8(5) . . . . ? C10 C9 O1 C13 22.7(18) . . . . ? C10 C9 O1A C13A -42(3) . . . . ? C10 C11 C12 C13 -6.8(8) . . . . ? C10 C11 C12 C13A 18.0(16) . . . . ? C10 C11 C12 C14 -178.9(4) . . . . ? C11 C12 C13 O1 23.4(15) . . . . ? C11 C12 C13A O1A -44(3) . . . . ? C11 C12 C14 C15 178.5(4) . . . . ? C12 C13 O1 C9 -31(2) . . . . ? C12 C13A O1A C9 56(4) . . . . ? C12 C14 C15 C16 -174.5(4) . . . . ? C13 C12 C14 C15 6.4(9) . . . . ? C13A C12 C14 C15 -20.0(18) . . . . ? C14 C12 C13 O1 -164.5(10) . . . . ? C14 C12 C13A O1A 153.7(18) . . . . ? C14 C15 C16 C17 3.4(6) . . . . ? C14 C15 C16 N1 -178.9(4) . . . . ? C15 C16 C17 C18 175.7(3) . . . . ? C15 C16 C17 C24 -67.8(4) . . . . ? C15 C16 C17 C25 55.8(5) . . . . ? C15 C16 N1 C19 -175.9(3) . . . . ? C15 C16 N1 C26 4.9(5) . . . . ? C16 C17 C18 C19 1.6(4) . . . . ? C16 C17 C18 C23 -179.9(4) . . . . ? C17 C16 N1 C19 2.1(4) . . . . ? C17 C16 N1 C26 -177.1(3) . . . . ? C17 C18 C19 C20 179.0(3) . . . . ? C17 C18 C19 N1 -0.5(4) . . . . ? C17 C18 C23 C22 -178.6(4) . . . . ? C18 C19 C20 C21 0.1(6) . . . . ? C18 C19 N1 C16 -1.0(4) . . . . ? C18 C19 N1 C26 178.2(3) . . . . ? C19 C18 C23 C22 -0.3(6) . . . . ? C19 C20 C21 C22 -0.4(6) . . . . ? C20 C19 N1 C16 179.5(4) . . . . ? C20 C19 N1 C26 -1.3(5) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C18 0.0(6) . . . . ? C23 C18 C19 C20 0.3(5) . . . . ? C23 C18 C19 N1 -179.2(3) . . . . ? C24 C17 C18 C19 -115.1(3) . . . . ? C24 C17 C18 C23 63.3(5) . . . . ? C25 C17 C18 C19 121.4(3) . . . . ? C25 C17 C18 C23 -60.1(5) . . . . ? C26 C27 C28 S1 -80.0(3) . . . . ? C27 C26 N1 C16 -91.1(4) . . . . ? C27 C26 N1 C19 89.8(4) . . . . ? C27 C28 S1 O2 66.0(3) . . . . ? C27 C28 S1 O3 -53.8(3) . . . . ? C27 C28 S1 O4 -174.0(3) . . . . ? N1 C16 C17 C18 -2.2(4) . . . . ? N1 C16 C17 C24 114.3(3) . . . . ? N1 C16 C17 C25 -122.1(3) . . . . ? N1 C19 C20 C21 179.4(3) . . . . ? N1 C26 C27 C28 163.8(3) . . . . ? O1 C9 C10 C5 175.8(7) . . . . ? O1 C9 C10 C11 -4.2(8) . . . . ? O1A C9 C10 C5 -164.1(12) . . . . ? O1A C9 C10 C11 15.9(13) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 2 10068.6 152.126 4 0 0 3 -7.08002 14.2684 4 0 0 -4 87.1955 27.1998 8 0 0 4 91.0516 27.0005 4 0 0 5 -9.79103 22.4795 4 0 0 -6 821.979 98.7054 6 0 0 -6 663.077 79.1754 8 0 0 6 844.506 84.95 4 0 0 7 1.68075 27.1709 4 0 0 -7 -96.6702 48.1496 6 0 0 -8 6716.38 322.825 6 0 0 -9 -5.97498 42.0352 6 0 0 -10 2765.69 236.087 6 0 0 11 -25.8182 52.1867 9 0 0 -11 3.27337 43.0004 6 0 0 12 19068.9 798.278 9 0 0 -12 18582.3 689.494 6 0 0 -13 -2.85882 35.7564 6 0 0 -14 324.397 35.4073 23 0 0 -15 11.0783 15.8688 23 0 0 -16 3533.95 111.921 14 0 0 -17 -10.7466 18.239 14 0 0 -18 -4.71659 17.1532 14 0 0 -19 9.60453 17.885 14 0 0 -20 868.679 49.9756 14 0 0 -21 -6.06509 11.0501 14 0 1 2 3621.95 100.39 4 0 -1 -2 3576.9 89.3825 8 0 -1 -2 3688.47 126.25 2 0 -1 3 44654.4 431.966 4 0 1 3 43813.7 404.925 4 0 1 4 102.494 27.9237 4 0 -1 4 71.0943 27.238 4 0 -1 -4 63.551 23.8858 8 0 1 -5 7977.27 244.537 8 0 -1 5 7663.66 232.938 4 0 1 5 7269.53 216.216 4 0 -1 -5 8005.05 279.349 5 0 -1 -6 10616.6 348.725 6 0 1 6 10326.6 285.762 4 0 1 -6 10565.1 315.319 8 0 -1 -6 11241.7 359.713 5 0 -1 6 10563.5 303.289 4 0 1 7 4175.66 199.832 4 0 1 -7 4843.43 260.245 6 0 -1 7 4751.92 225.835 4 0 -1 -7 4982.85 266.631 6 0 1 -8 6944.06 329.096 6 0 1 8 6464.11 349.742 9 0 -1 -8 6447.31 316.376 6 0 -1 8 6315.7 280.106 4 0 1 9 13192.6 541.052 9 0 -1 -9 13540.9 492.037 6 0 1 -9 13037.7 480.811 6 0 1 10 13075.8 584.503 9 0 -1 -10 13128.6 516.309 6 0 1 -10 12708.2 505.541 6 0 -1 -11 6494.74 390.313 6 0 1 11 7033.83 459.136 9 0 1 -11 6748.88 391.878 6 0 1 -12 709.61 136.373 6 0 -1 -12 390.725 110.219 6 0 -1 12 587.817 145.634 9 0 -1 -13 460.396 124.823 6 0 1 -13 514.466 131.195 6 0 -1 -14 185.603 28.8487 23 0 1 -14 142.957 24.476 23 0 -1 -14 148.878 25.2534 13 0 -1 -15 1775.23 80.1826 23 0 1 -15 1796.87 78.5836 14 0 -1 -15 1735.67 78.5546 13 0 -1 -16 559.979 47.0323 13 0 -1 -16 572.903 46.7064 14 0 1 -16 546.166 45.9167 14 0 1 -17 753.931 52.9552 14 0 -1 -17 717.303 52.6398 13 0 -1 -17 805.398 55.8992 14 0 -1 -18 535.727 45.5609 14 0 1 -18 511.2 43.792 14 0 1 -19 13.9432 15.9349 14 0 -1 -19 -5.80593 15.8952 14 0 1 -20 192.406 25.6557 14 0 -1 -20 185.899 27.156 14 0 -1 -21 -12.4445 12.7171 14 0 1 -21 0.8019 11.5088 14 0 -2 0 367.294 30.9845 3 0 -2 -1 390.745 42.951 2 0 -2 -1 349.167 34.1455 3 0 -2 -2 40915 457.769 2 0 -2 -2 41203.3 364.227 7 0 -2 -3 53173.3 600.034 2 0 2 3 52518.4 660.869 9 0 2 3 53162.9 439.342 4 0 2 4 14184.7 265.777 4 0 2 4 14393.4 374.913 9 0 -2 -4 14340.7 353.792 2 0 -2 4 13932.5 295.943 4 0 2 5 13568.7 287.796 4 0 -2 5 13480.7 324.347 4 0 2 5 13428.4 398.066 9 0 -2 -5 13889.6 364.754 5 0 -2 6 37608.2 594.686 4 0 2 6 36109.1 711.382 9 0 -2 -6 38699.9 671.855 5 0 2 6 36327.9 512.78 4 0 -2 -6 37201.4 642.456 6 0 2 -6 37244.6 598.929 8 0 2 -7 5296.14 249.883 8 0 -2 -7 5304.02 270.38 6 0 -2 7 5529.56 253.211 4 0 -2 -7 5349.8 274.772 5 0 2 7 5296.2 208.499 4 0 2 7 5444.85 303.862 9 0 2 8 8563.43 412.78 9 0 2 -8 8851.39 369.268 6 0 -2 8 8371.83 333.674 4 0 -2 -8 8634.02 369.059 6 0 2 9 7427.33 421.755 9 0 -2 9 7793.5 307.724 11 0 2 -9 8341.23 380.876 6 0 -2 -9 7261.11 368.506 6 0 2 -10 2048.63 204.627 6 0 2 10 2504.88 263.138 9 0 -2 -10 2192 216.994 6 0 2 11 964.35 174.314 9 0 -2 -11 855.768 146.427 6 0 2 -11 1104.3 160.932 6 0 -2 -12 392.264 110.689 6 0 2 -12 461.06 112.41 6 0 -2 -13 1584.5 223.104 6 0 2 -13 1748.42 222.92 6 0 -2 -14 63.6789 18.1131 13 0 2 -14 99.2735 21.7985 23 0 -2 -14 97.8275 23.2441 23 0 2 -15 -9.91752 18.2506 14 0 -2 -15 -9.70376 17.3274 23 0 -2 -15 1.51088 16.4566 13 0 -2 -16 151.318 27.7234 14 0 -2 -16 138.846 27.9531 13 0 2 -16 123.341 25.0027 14 0 -2 -17 5616.7 142.391 13 0 2 -17 5826.76 140.013 14 0 -2 -17 5747.16 142.777 14 0 2 -18 -3.83234 18.1038 14 0 -2 -18 13.8871 18.6909 13 0 -2 -18 12.0847 16.8178 14 0 -2 -19 182.619 29.1517 14 0 2 -19 207.957 27.4736 14 0 -2 -20 321.16 33.8458 14 0 -2 -21 -17.8329 15.6529 14 0 3 0 45.6422 9.58444 8 0 -3 0 78.5334 21.4633 3 0 -3 -1 24153.3 365.233 2 0 -3 -1 24571.6 320.464 3 0 3 -1 24469.6 266.214 8 0 3 -2 12405.6 213.711 10 0 -3 -2 12595.9 217.013 7 0 -3 -2 11861.8 237.638 6 0 3 -3 5872.68 175.718 10 0 -3 -3 5525.33 210.209 2 0 -3 -3 5294.44 178.295 6 0 -3 -3 5693.04 207.226 5 0 -3 -4 2665.16 162.701 2 0 3 4 2566.61 184.519 9 0 -3 -4 2426.78 136.808 6 0 -3 5 14095 352.414 4 0 3 5 14041 444.88 9 0 -3 -5 14388.8 367.905 6 0 -3 -5 14571.2 406.541 2 0 -3 -5 14652.3 385.05 5 0 -3 6 9118.14 308.885 4 0 -3 -6 8912.59 322.329 6 0 3 -6 9566.34 312.759 8 0 -3 -6 9131.8 332.196 5 0 3 6 9257.95 380.659 9 0 3 7 2437.16 213.248 9 0 -3 7 2296.28 170.7 4 0 -3 -7 2529.43 189.688 5 0 -3 -7 2516.48 188.015 6 0 3 -7 2343.53 172.329 8 0 -3 8 149.534 47.7496 11 0 -3 8 113.589 49.6181 4 0 3 -8 150.04 59.8934 6 0 -3 -8 168.212 62.3778 6 0 -3 -8 220.228 72.7299 5 0 3 8 108.776 66.2279 9 0 3 -9 13718.9 489.592 6 0 -3 -9 12977.3 498.784 6 0 3 9 13731.8 574.831 9 0 -3 9 12836.7 461.253 4 0 -3 9 12809.2 409.653 11 0 3 10 2606.17 271.04 9 0 -3 -10 2677.83 242.778 6 0 3 -10 2995.77 247.422 6 0 3 -11 11730.8 514.543 6 0 -3 -11 10566.4 511.01 6 0 3 -12 3871.99 315.56 6 0 -3 -12 4106.03 343.23 6 0 3 -13 1486.48 206.897 6 0 -3 -13 1574.57 223.654 6 0 -3 -14 394.744 38.8054 23 0 -3 -14 374.026 37.6412 13 0 -3 -15 347.856 38.9673 23 0 3 -15 390.703 36.6451 14 0 -3 -15 366.415 38.4295 13 0 -3 -16 0.53998 20.6985 14 0 3 -16 11.3893 15.3188 14 0 -3 -16 45.382 21.3184 23 0 -3 -16 6.00011 16.5395 13 0 -3 -17 710.908 53.5772 13 0 3 -17 735.069 50.4808 14 0 -3 -17 668.524 51.7039 14 0 -3 -18 50.3731 20.7969 14 0 -3 -18 34.1711 17.9192 13 0 3 -18 47.5638 18.406 14 0 -3 -19 35.4562 18.5984 13 0 -3 -19 68.1984 22.3763 14 0 -3 -20 123.543 24.4515 14 0 -3 -21 130.123 20.6945 14 0 4 0 34962.6 264.584 8 0 -4 0 36362 420.562 3 0 -4 -1 38251.8 458.519 3 0 4 -1 38280.9 362.963 8 0 -4 -1 37413 511.749 2 0 -4 -2 15383.5 272.319 7 0 4 -2 15607.9 274.587 8 0 -4 -2 15084.6 310.586 3 0 -4 -3 179.714 46.7311 5 0 4 -3 230.088 43.3004 8 0 4 -3 183.146 36.4948 10 0 -4 -3 160.817 41.414 6 0 -4 -3 186.863 51.3786 2 0 -4 -3 188.668 36.1894 7 0 -4 4 7693.07 253.827 11 0 -4 -4 7432.21 250.874 6 0 -4 -4 7863.62 284.069 2 0 4 -5 2305.01 147.213 8 0 4 -5 2196.54 139.724 10 0 -4 -5 2284.79 158.117 5 0 -4 -5 2301.31 155.227 6 0 -4 -5 2085.27 162.535 2 0 -4 5 2350.48 152.328 11 0 4 5 2614.74 205.717 9 0 -4 -6 20.2591 28.4353 5 0 -4 -6 23.3169 39.4915 6 0 4 -6 23.6139 30.5556 8 0 -4 6 16.6768 28.4494 4 0 4 6 20.3668 51.781 9 0 -4 6 53.1551 36.9774 11 0 -4 -6 69.1544 46.2465 2 0 4 7 1807.65 199.689 9 0 -4 -7 1886.84 167.593 5 0 -4 7 1696.59 144.281 11 0 -4 -7 1793.47 164.553 6 0 4 -7 1749.57 152.162 8 0 -4 7 1602.16 150.445 4 0 -4 8 591.027 94.2871 11 0 -4 8 543.198 97.323 4 0 -4 -8 560.897 101.875 5 0 4 8 722.303 141.692 9 0 -4 -8 486.402 103.007 6 0 -4 -9 270.295 80.4477 6 0 -4 -9 307.822 87.7954 5 0 -4 9 278.585 72.3379 11 0 4 9 327.22 107.883 9 0 -4 9 344.857 86.9112 4 0 4 -9 209.114 72.154 6 0 -4 -10 3010.08 264.389 6 0 4 10 3151.62 302.743 9 0 4 -10 3259.83 259.783 6 0 -4 -11 6009.15 394.342 6 0 4 -11 5974.44 369.529 6 0 4 -12 821.944 148.982 6 0 -4 -12 786.772 156.11 6 0 4 -13 3780.69 327.891 6 0 -4 -13 5289.92 413.599 6 0 -4 -14 40.9034 17.65 13 0 -4 -14 29.392 17.0452 23 0 4 -14 34.5152 16.5689 16 0 -4 -15 3631.93 113.451 23 0 -4 -15 3507.81 111.205 14 0 -4 -15 3472.49 111.535 13 0 -4 -16 119.347 26.2429 14 0 -4 -16 144.843 28.2087 13 0 -4 -16 188.869 31.6554 23 0 -4 -17 404.807 41.8411 13 0 -4 -17 344.621 37.5125 14 0 -4 -18 252.175 32.4834 14 0 -4 -18 292.241 35.9813 13 0 -4 -19 202.899 28.9855 13 0 -4 -19 249.039 32.7474 14 0 -4 -20 65.3828 21.1226 14 0 -4 -20 41.9812 17.0719 13 0 -4 -21 281.904 28.2476 14 0 5 0 16.9562 11.336 8 0 -5 0 3.16588 28.8804 11 0 -5 0 -4.88087 27.534 3 0 -5 -1 20863.8 373.414 3 0 5 -1 20919.2 289.034 8 0 -5 -1 20211.3 419.393 2 0 -5 -2 34750.2 514.75 3 0 -5 -2 35181.8 466.146 7 0 5 -2 35371.5 436.477 8 0 5 -3 37075.3 465.078 10 0 -5 -3 36304.5 484.623 7 0 -5 -3 36236 621.58 2 0 5 -3 36784.5 502.679 8 0 5 -4 40855.6 580.018 8 0 -5 -4 40321.8 674.92 2 0 -5 4 41031.7 622.933 11 0 -5 -4 40855.7 660.805 5 0 -5 -4 39038.9 610.918 6 0 -5 5 14563.6 401.695 11 0 -5 -5 15068.1 420.437 5 0 5 -5 15038.5 381.712 10 0 -5 -5 14827.2 407.741 6 0 -5 -5 14494 440.671 2 0 5 -5 15153.1 386.505 8 0 -5 6 9689.31 337.272 11 0 -5 -6 9849.18 356.831 5 0 -5 -6 9892.07 358.615 6 0 -5 -6 9433.37 375.407 2 0 -5 6 9528.58 354.529 4 0 5 -6 9314.35 333.78 8 0 5 7 1803.16 199.657 9 0 5 -7 1638.5 151.528 8 0 -5 -7 1571.22 156.81 6 0 -5 -7 1436.23 150.191 5 0 -5 7 1469.43 141.151 11 0 -5 7 1510.65 152.712 4 0 5 8 8414.41 447.695 9 0 -5 8 8405.19 375.593 4 0 -5 8 8517.29 351.625 11 0 -5 -8 8073.18 371.916 5 0 -5 -8 8297.19 384.292 6 0 5 -9 317.797 82.6917 6 0 5 9 346.665 102.764 9 0 -5 9 259.638 77.7729 4 0 -5 9 295.323 79.6734 11 0 -5 -9 323.954 86.5195 5 0 -5 -9 306.19 85.9899 6 0 -5 -10 5911.64 375.149 6 0 5 -10 6271.24 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7.11696 13.8016 23 -2 -7 12 -33.8708 57.491 4 -2 -7 11 3872.01 361.581 4 2 7 -10 603.627 128.512 10 -2 -7 10 845.092 166.059 4 2 7 -9 917.041 150.701 10 -2 -7 9 977.742 169.632 4 2 7 -8 433.321 102.285 10 -2 -7 8 274.951 79.4742 7 -2 -7 8 321.94 103.44 4 2 7 -7 53.7915 44.5086 10 -2 -7 7 70.2205 59.6239 4 -2 -7 7 68.3818 52.1713 7 -2 -7 6 4572.62 309.07 4 -2 -7 6 4309.28 270.897 7 -2 -7 5 1267.79 157.082 4 -2 -7 5 1424.25 154.394 7 -2 -7 4 1781.77 175.762 4 -2 -7 4 1803.67 171.272 7 -2 -7 3 7948.05 343.04 4 -2 -7 3 7783.95 350.162 7 -2 -7 2 27969.6 608.801 4 -2 -7 2 29054.6 677.676 7 2 -7 -2 27865.2 506.652 11 -2 -7 1 2602.74 179.567 4 -2 -7 1 2664.35 210.408 7 -2 -7 0 3933.83 209.824 4 -2 -7 0 3746.57 249.787 7 -2 -7 -1 55.9419 63.2774 7 -2 -7 -1 226.701 96.5413 2 -2 -7 -1 130.476 44.6483 4 -2 -7 -2 491.192 100.42 3 -2 -7 -2 461.5 114.728 2 -2 -7 -3 465.022 98.3805 3 -2 -7 -3 502.366 116.025 2 -2 -7 -4 1454.48 195.734 2 -2 -7 -4 1259.92 156.147 3 -2 -7 -4 1118.17 165.663 5 -2 7 -5 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76.2154 7 2 -8 -3 125.984 39.5889 11 -2 -8 3 127.614 60.3361 4 -2 -8 2 9210.29 398.869 7 -2 -8 2 9248.42 367.89 4 2 -8 -2 8865.82 304.228 11 -2 -8 1 17541.8 481.931 4 -2 -8 1 17916.6 559.032 7 2 -8 -1 17050.3 451.08 11 -2 -8 0 240.142 61.5552 4 -2 -8 0 79.1547 63.9568 7 -2 -8 -1 1475.29 130.535 4 -2 -8 -1 1386.59 165.165 3 -2 -8 -1 1564.94 175.525 7 -2 -8 -1 1442.9 192.025 2 -2 -8 -2 9415.79 470.667 2 -2 -8 -2 9754.1 312.83 4 -2 -8 -2 9778.54 426.24 3 -2 -8 -2 9630.28 428.939 7 -2 -8 -3 126.446 83.6299 2 -2 -8 -3 71.6758 53.515 3 -2 8 -4 631.011 108.862 8 -2 -8 -4 593.091 138.371 2 -2 -8 -4 670.901 119.126 3 -2 8 -5 4001 265.407 8 -2 -8 -5 3986.76 321.056 2 -2 -8 -5 3728.35 306.101 5 -2 -8 -5 3953.75 286.746 3 -2 8 -6 597.124 113.195 8 -2 -8 -6 617.164 130.877 5 -2 -8 -6 579.63 131.555 2 -2 -8 -7 586.636 128.922 2 -2 8 -7 452.485 104.116 8 -2 -8 -7 470.528 119.978 5 -2 8 -8 1950.01 215.295 8 -2 -8 -8 1748.96 227.594 2 -2 -8 -8 2390.87 263.571 5 -2 -8 -9 79.6554 56.8869 2 -2 8 -9 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36.5302 13 2 -10 -15 -1.79692 16.7198 23 2 -10 -14 12.3313 17.1249 23 2 -10 -13 1796.98 79.4533 23 2 10 -13 1763.12 83.1199 20 2 -10 -12 1779.65 78.6479 23 2 10 -12 1861.74 82.8042 20 2 -10 -11 10751.7 184.14 23 2 10 -11 10626.8 186.549 20 2 10 -10 125.725 61.889 10 -2 -10 10 165.208 91.0778 4 -2 -10 9 1725.58 236.163 4 -2 -10 9 1938.03 229.381 7 2 10 -8 230.425 88.4453 10 -2 -10 8 94.8949 79.6964 4 -2 -10 8 66.6662 55.903 7 2 10 -7 2912.19 255.01 10 -2 -10 7 2579.68 269.271 4 -2 -10 7 2972.89 271.388 7 -2 -10 6 2450.16 256.828 4 -2 -10 6 2090.55 228.097 7 -2 -10 5 281.319 96.0003 7 -2 -10 5 375.603 102.602 4 -2 -10 4 19.5463 47.3445 4 -2 -10 4 57.9371 52.0444 7 -2 -10 3 15961.4 557.571 4 -2 -10 3 16310.3 588.247 7 -2 -10 2 9412.66 445.067 7 -2 -10 2 9721.6 417.674 4 2 -10 -2 9194.22 354.117 11 -2 -10 1 885.336 127.366 4 -2 -10 1 661.355 129.871 7 2 -10 -1 807.551 113.97 11 -2 -10 0 10101.4 389.725 4 -2 -10 0 10093.4 469.729 7 -2 -10 0 9277.26 448.964 3 2 -10 0 10255.4 413.296 11 -2 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284.066 91.9933 8 -2 -10 -9 236.039 91.4637 5 2 -10 9 227.572 91.1469 11 -2 -10 -10 51.5601 17.986 13 -2 -10 -10 47.1657 19.5184 15 -2 -10 -10 51.0641 19.4433 14 -2 10 -10 61.8178 21.2795 16 -2 -10 -11 1467.05 74.1685 15 -2 -10 -11 1474.27 76.7212 14 -2 -10 -11 1446.41 73.0342 13 -2 10 -11 1501.29 71.2067 16 -2 -10 -12 33.7115 20.6397 13 -2 10 -12 48.6596 22.389 16 -2 -10 -12 39.2773 21.2569 14 -2 -10 -13 4978.04 142.807 14 -2 10 -13 5177.19 132.991 16 -2 -10 -13 5030.87 138.438 13 -2 -10 -14 98.9085 26.8394 13 -2 -10 -14 81.2635 24.4506 14 -2 10 -14 117.874 25.7747 16 -2 -10 -15 2323.02 96.2204 13 -2 -10 -15 2377.1 96.9866 14 -2 10 -15 2372.76 89.627 16 -2 -10 -16 -19.3757 23.6683 14 -2 -10 -16 10.9515 20.6229 13 -2 10 -16 9.47358 18.7872 16 -2 -10 -17 664.223 50.2825 14 -2 -10 -17 691.532 50.3368 13 -2 10 -17 701.279 45.6314 16 -2 -10 -18 49.6241 20.0997 13 -2 -10 -18 55.8649 22.1603 14 2 -11 -19 94.1116 19.0079 13 2 -11 -19 80.384 18.0913 14 2 -11 -18 185.486 27.2376 13 2 -11 -18 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