#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:41:05 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227294 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035893.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_4035893 loop_ _publ_author_name 'Ma, Yan-Na' 'Bian, Yajing' 'Liu, Xin' 'Zhang, Jie' 'Chen, Xuenian' _publ_section_title ; One-Pot Synthesis of Iodo-Dibenzothiazines from 2-Biaryl Sulfides. ; _journal_issue 1 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 450 _journal_page_last 457 _journal_paper_doi 10.1021/acs.joc.8b02729 _journal_volume 84 _journal_year 2019 _chemical_formula_moiety 'C14 H11 I2 N O S' _chemical_formula_sum 'C14 H11 I2 N O S' _chemical_formula_weight 495.10 _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 dual _audit_creation_date 2018-08-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 99.157(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.4188(3) _cell_length_b 5.00910(10) _cell_length_c 20.2178(3) _cell_measurement_reflns_used 5602 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 71.8300 _cell_measurement_theta_min 4.4080 _cell_volume 1541.61(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _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 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0528 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -105.00 -17.00 1.00 1.00 -- -35.50 -38.00 -60.00 88 2 \w -105.00 -17.00 1.00 1.00 -- -35.50 -38.00-150.00 88 3 \w 19.00 103.00 1.00 1.00 -- 35.50 57.00-180.00 84 4 \w 23.00 89.00 1.00 1.00 -- 35.50-125.00 0.00 66 5 \w 23.00 89.00 1.00 1.00 -- 35.50-125.00 -60.00 66 6 \w -36.00 65.00 1.00 1.00 -- 35.50 -19.00-150.00 101 7 \w -32.00 52.00 1.00 1.00 -- 35.50 -57.00-150.00 84 8 \w 9.00 103.00 1.00 1.00 -- 35.50 77.00 -60.00 94 9 \w 39.00 109.00 1.00 2.40 -- 108.69 -95.00-120.00 70 10 \w 39.00 130.00 1.00 2.40 -- 108.69 -30.00 150.00 91 11 \w 39.00 114.00 1.00 2.40 -- 108.69-115.00 52.00 75 12 \w 70.00 178.00 1.00 2.40 -- 108.69 15.00-120.00 108 13 \w 39.00 130.00 1.00 2.40 -- 108.69 -30.00-120.00 91 14 \w 91.00 176.00 1.00 2.40 -- 108.69 61.00 -60.00 85 15 \w 39.00 109.00 1.00 2.40 -- 108.69 -95.00 90.00 70 16 \w -103.00 -9.00 1.00 1.00 -- -35.50 -77.00 60.00 94 17 \w -106.00 -43.00 1.00 1.00 -- -35.50-168.00 -91.00 63 18 \w -32.00 62.00 1.00 1.00 -- 35.50 -77.00 120.00 94 19 \w 1.00 74.00 1.00 1.00 -- 35.50 -99.00 120.00 73 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0947593000 _diffrn_orient_matrix_UB_12 0.1081744000 _diffrn_orient_matrix_UB_13 0.0098434000 _diffrn_orient_matrix_UB_21 -0.0097766000 _diffrn_orient_matrix_UB_22 0.0603338000 _diffrn_orient_matrix_UB_23 -0.0755570000 _diffrn_orient_matrix_UB_31 -0.0343461000 _diffrn_orient_matrix_UB_32 0.2812581000 _diffrn_orient_matrix_UB_33 0.0123865000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_unetI/netI 0.0628 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 8835 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.085 _diffrn_reflns_theta_min 4.430 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 33.241 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.05543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.133 _exptl_crystal_description block _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.142 _refine_diff_density_min -1.738 _refine_diff_density_rms 0.205 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2965 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.054 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0598 _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^)+(0.1021P)^2^+0.5992P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1587 _refine_ls_wR_factor_ref 0.1688 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2473 _reflns_number_total 2965 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL myn-20180731_a.res in P2(1)/c myn-20180731.res created by SHELXL-2016/6 at 18:13:54 on 01-Aug-2018 REM Old TITL myn-20180731 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.198, Rweak 0.018, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C14 O S I2 N CELL 1.54184 15.4188 5.0091 20.2178 90 99.157 90 ZERR 4 0.0003 0.0001 0.0003 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O S UNIT 56 44 8 4 4 4 L.S. 10 PLAN 20 BOND $H LIST 6 fmap 2 acta REM REM REM WGHT 0.102100 0.599200 FVAR 0.29144 I1 3 0.540034 -0.247594 0.644499 11.00000 0.04043 0.06990 = 0.07702 0.01337 0.01322 0.01626 I2 3 0.225225 -0.050929 0.775555 11.00000 0.04861 0.08492 = 0.03764 0.01969 0.01111 -0.00144 S1 6 0.121087 0.427766 0.584559 11.00000 0.03066 0.02992 = 0.03485 0.00290 0.00617 -0.00060 O1 5 0.059851 0.251745 0.543151 11.00000 0.03871 0.02741 = 0.05262 -0.00008 -0.00024 -0.00172 N1 4 0.177618 0.312686 0.648304 11.00000 0.03316 0.04650 = 0.03646 0.00841 0.00965 -0.00248 C1 1 0.193571 0.565675 0.535189 11.00000 0.04107 0.02645 = 0.02756 0.00133 0.00786 -0.00842 C2 1 0.163022 0.760169 0.487462 11.00000 0.05319 0.03584 = 0.03228 0.00283 0.00479 0.00101 AFIX 43 H2 2 0.106087 0.826135 0.483897 11.00000 -1.20000 AFIX 0 C3 1 0.219588 0.852601 0.445515 11.00000 0.06889 0.04979 = 0.03584 0.01106 0.01122 -0.00794 AFIX 43 H3 2 0.201122 0.982510 0.413497 11.00000 -1.20000 AFIX 0 C4 1 0.303525 0.749407 0.451903 11.00000 0.06170 0.05167 = 0.03333 0.00433 0.01500 -0.01259 AFIX 43 H4 2 0.341380 0.811837 0.423874 11.00000 -1.20000 AFIX 0 C5 1 0.332765 0.555701 0.498880 11.00000 0.04161 0.05801 = 0.03158 0.00570 0.01071 -0.00452 AFIX 43 H5 2 0.389646 0.489942 0.501744 11.00000 -1.20000 AFIX 0 C6 1 0.277427 0.456000 0.542670 11.00000 0.03925 0.03309 = 0.02960 0.00206 0.00657 -0.00989 C7 1 0.309053 0.253154 0.594114 11.00000 0.03210 0.03540 = 0.02811 -0.00027 0.00525 -0.00240 C8 1 0.388386 0.118353 0.594300 11.00000 0.03367 0.04375 = 0.04113 0.00298 0.00809 0.00260 AFIX 43 H8 2 0.421073 0.150540 0.560232 11.00000 -1.20000 AFIX 0 C9 1 0.418923 -0.060987 0.643977 11.00000 0.03314 0.04006 = 0.04316 0.00230 -0.00064 0.01158 C10 1 0.371116 -0.113937 0.694410 11.00000 0.03567 0.05499 = 0.03808 0.00301 -0.00251 -0.00012 AFIX 43 H10 2 0.391917 -0.234883 0.728123 11.00000 -1.20000 AFIX 0 C11 1 0.292800 0.013102 0.694390 11.00000 0.03416 0.04093 = 0.03322 0.00463 0.00443 -0.00502 C12 1 0.257491 0.195813 0.644089 11.00000 0.03459 0.02489 = 0.03201 0.00394 0.00646 -0.00588 C13 1 0.060102 0.690090 0.613677 11.00000 0.05364 0.02008 = 0.05237 -0.00662 0.01642 0.00259 AFIX 23 H13A 2 0.099897 0.823663 0.636082 11.00000 -1.20000 H13B 2 0.023399 0.774522 0.576047 11.00000 -1.20000 AFIX 0 C14 1 0.002817 0.579941 0.662219 11.00000 0.06192 0.06121 = 0.07557 -0.00548 0.03970 -0.00239 AFIX 137 H14A 2 -0.038062 0.453082 0.639385 11.00000 -1.50000 H14B 2 -0.028832 0.723611 0.678867 11.00000 -1.50000 H14C 2 0.039269 0.493760 0.698977 11.00000 -1.50000 AFIX 0 HKLF 4 REM myn-20180731_a.res in P2(1)/c REM R1 = 0.0598 for 2473 Fo > 4sig(Fo) and 0.0765 for all 2965 data REM 173 parameters refined using 0 restraints END WGHT 0.1019 0.6824 REM Highest difference peak 1.142, deepest hole -1.738, 1-sigma level 0.205 Q1 1 0.5713 -0.2517 0.5921 11.00000 0.05 1.14 Q2 1 0.1900 -0.0567 0.8238 11.00000 0.05 1.01 Q3 1 0.5664 -0.4258 0.6417 11.00000 0.05 0.95 Q4 1 0.5092 -0.2440 0.6919 11.00000 0.05 0.94 Q5 1 0.5236 -0.0564 0.6478 11.00000 0.05 0.85 Q6 1 0.2434 0.1355 0.7758 11.00000 0.05 0.79 Q7 1 0.2476 -0.2444 0.7713 11.00000 0.05 0.78 Q8 1 0.5090 -0.4382 0.6418 11.00000 0.05 0.77 Q9 1 0.2199 0.1544 0.7780 11.00000 0.05 0.77 Q10 1 0.2611 -0.0650 0.7213 11.00000 0.05 0.77 Q11 1 0.2115 -0.1642 0.6787 11.00000 0.05 0.72 Q12 1 0.5364 -0.1279 0.7392 11.00000 0.05 0.70 Q13 1 0.1647 0.4485 0.5396 11.00000 0.05 0.67 Q14 1 0.2305 0.0754 0.8683 11.00000 0.05 0.66 Q15 1 0.0977 0.4385 0.7270 11.00000 0.05 0.63 Q16 1 0.2078 -0.2475 0.7781 11.00000 0.05 0.63 Q17 1 0.6472 -0.0602 0.6747 11.00000 0.05 0.63 Q18 1 0.5407 -0.3794 0.7379 11.00000 0.05 0.62 Q19 1 0.2404 0.6619 0.3679 11.00000 0.05 0.59 Q20 1 0.4086 -0.5007 0.6803 11.00000 0.05 0.58 REM The information below was added by Olex2. REM REM R1 = 0.0598 for 2473 Fo > 4sig(Fo) and 0.0765 for all 9657 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.14, deepest hole -1.74 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0765 REM R1_gt = 0.0598 REM wR_ref = 0.1688 REM GOOF = 1.054 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 9657 REM Reflections_gt = 2473 REM Parameters = n/a REM Hole = -1.74 REM Peak = 1.14 REM Flack = n/a ; _cod_data_source_file jo8b02729_si_002.cif _cod_data_source_block myn-20180731 _cod_database_code 4035893 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C1 H1 O1 S1 I1' _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. ; _reflns_odcompleteness_completeness 99.61 _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.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10) 2.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 6.702 _oxdiff_exptl_absorpt_empirical_full_min 0.453 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 I1 I 0.54003(4) -0.24759(13) 0.64450(3) 0.0620(3) Uani 1 1 d . I2 I 0.22523(4) -0.05093(14) 0.77555(2) 0.0566(3) Uani 1 1 d . S1 S 0.12109(11) 0.4278(4) 0.58456(8) 0.0317(4) Uani 1 1 d . O1 O 0.0599(4) 0.2517(10) 0.5432(3) 0.0404(12) Uani 1 1 d . N1 N 0.1776(4) 0.3127(14) 0.6483(3) 0.0383(14) Uani 1 1 d . C1 C 0.1936(5) 0.5657(14) 0.5352(3) 0.0314(15) Uani 1 1 d . C2 C 0.1630(6) 0.7602(15) 0.4875(3) 0.0407(18) Uani 1 1 d . H2 H 0.106087 0.826135 0.483897 0.049 Uiso 1 1 calc R C3 C 0.2196(6) 0.853(2) 0.4455(4) 0.051(2) Uani 1 1 d . H3 H 0.201122 0.982510 0.413497 0.061 Uiso 1 1 calc R C4 C 0.3035(6) 0.7494(16) 0.4519(4) 0.048(2) Uani 1 1 d . H4 H 0.341380 0.811837 0.423874 0.058 Uiso 1 1 calc R C5 C 0.3328(5) 0.5557(17) 0.4989(3) 0.0432(18) Uani 1 1 d . H5 H 0.389646 0.489942 0.501744 0.052 Uiso 1 1 calc R C6 C 0.2774(5) 0.4560(15) 0.5427(3) 0.0339(15) Uani 1 1 d . C7 C 0.3091(5) 0.2532(14) 0.5941(3) 0.0318(15) Uani 1 1 d . C8 C 0.3884(5) 0.1184(17) 0.5943(3) 0.0393(17) Uani 1 1 d . H8 H 0.421073 0.150540 0.560232 0.047 Uiso 1 1 calc R C9 C 0.4189(5) -0.0610(16) 0.6440(4) 0.0395(17) Uani 1 1 d . C10 C 0.3711(5) -0.1139(18) 0.6944(4) 0.0438(18) Uani 1 1 d . H10 H 0.391917 -0.234883 0.728123 0.053 Uiso 1 1 calc R C11 C 0.2928(5) 0.0131(16) 0.6944(3) 0.0362(16) Uani 1 1 d . C12 C 0.2575(5) 0.1958(14) 0.6441(3) 0.0304(14) Uani 1 1 d . C13 C 0.0601(6) 0.6901(15) 0.6137(4) 0.0412(17) Uani 1 1 d . H13A H 0.099897 0.823663 0.636082 0.049 Uiso 1 1 calc R H13B H 0.023399 0.774522 0.576047 0.049 Uiso 1 1 calc R C14 C 0.0028(7) 0.580(2) 0.6622(5) 0.063(3) Uani 1 1 d . H14A H -0.038062 0.453082 0.639385 0.095 Uiso 1 1 calc GR H14B H -0.028832 0.723611 0.678867 0.095 Uiso 1 1 calc GR H14C H 0.039269 0.493760 0.698977 0.095 Uiso 1 1 calc GR 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 I1 0.0404(4) 0.0699(5) 0.0770(4) 0.0134(3) 0.0132(3) 0.0163(3) I2 0.0486(4) 0.0849(5) 0.0376(3) 0.0197(2) 0.0111(2) -0.0014(3) S1 0.0307(8) 0.0299(10) 0.0349(7) 0.0029(6) 0.0062(6) -0.0006(7) O1 0.039(3) 0.027(3) 0.053(3) 0.000(2) 0.000(2) -0.002(2) N1 0.033(3) 0.046(4) 0.036(3) 0.008(3) 0.010(2) -0.002(3) C1 0.041(4) 0.026(4) 0.028(3) 0.001(3) 0.008(3) -0.008(3) C2 0.053(5) 0.036(5) 0.032(3) 0.003(3) 0.005(3) 0.001(4) C3 0.069(6) 0.050(5) 0.036(3) 0.011(4) 0.011(3) -0.008(5) C4 0.062(5) 0.052(5) 0.033(3) 0.004(3) 0.015(3) -0.013(4) C5 0.042(4) 0.058(5) 0.032(3) 0.006(3) 0.011(3) -0.005(4) C6 0.039(4) 0.033(4) 0.030(3) 0.002(3) 0.007(3) -0.010(3) C7 0.032(3) 0.035(4) 0.028(3) 0.000(3) 0.005(2) -0.002(3) C8 0.034(4) 0.044(5) 0.041(3) 0.003(3) 0.008(3) 0.003(3) C9 0.033(4) 0.040(5) 0.043(4) 0.002(3) -0.001(3) 0.012(3) C10 0.036(4) 0.055(5) 0.038(3) 0.003(3) -0.003(3) 0.000(4) C11 0.034(4) 0.041(5) 0.033(3) 0.005(3) 0.004(3) -0.005(3) C12 0.035(3) 0.025(4) 0.032(3) 0.004(3) 0.006(3) -0.006(3) C13 0.054(5) 0.020(4) 0.052(4) -0.007(3) 0.016(3) 0.003(3) C14 0.062(6) 0.061(7) 0.076(6) -0.005(5) 0.040(5) -0.002(5) 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' I I -0.3257 6.8362 '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 O1 S1 N1 118.8(3) O1 S1 C1 109.0(3) O1 S1 C13 108.1(4) N1 S1 C1 107.2(3) N1 S1 C13 105.0(4) C1 S1 C13 108.5(4) C12 N1 S1 119.8(5) C2 C1 S1 119.4(6) C6 C1 S1 116.6(5) C6 C1 C2 123.7(6) C1 C2 H2 120.7 C3 C2 C1 118.6(8) C3 C2 H2 120.7 C2 C3 H3 120.4 C4 C3 C2 119.2(8) C4 C3 H3 120.4 C3 C4 H4 119.1 C3 C4 C5 121.7(7) C5 C4 H4 119.1 C4 C5 H5 119.5 C4 C5 C6 121.0(8) C6 C5 H5 119.5 C1 C6 C5 115.8(7) C1 C6 C7 123.0(6) C5 C6 C7 121.2(7) C8 C7 C6 121.6(6) C8 C7 C12 119.5(6) C12 C7 C6 118.9(6) C7 C8 H8 119.5 C9 C8 C7 121.1(7) C9 C8 H8 119.5 C8 C9 I1 119.9(6) C8 C9 C10 120.4(7) C10 C9 I1 119.6(6) C9 C10 H10 120.4 C11 C10 C9 119.2(7) C11 C10 H10 120.4 C10 C11 I2 118.5(5) C10 C11 C12 122.8(7) C12 C11 I2 118.6(5) N1 C12 C7 124.6(6) N1 C12 C11 118.5(6) C7 C12 C11 116.8(6) S1 C13 H13A 109.7 S1 C13 H13B 109.7 H13A C13 H13B 108.2 C14 C13 S1 109.8(6) C14 C13 H13A 109.7 C14 C13 H13B 109.7 C13 C14 H14A 109.5 C13 C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C9 2.087(7) I2 C11 2.104(7) S1 O1 1.455(5) S1 N1 1.548(6) S1 C1 1.754(7) S1 C13 1.770(7) N1 C12 1.378(9) C1 C2 1.399(10) C1 C6 1.391(10) C2 H2 0.9300 C2 C3 1.389(11) C3 H3 0.9300 C3 C4 1.380(13) C4 H4 0.9300 C4 C5 1.382(11) C5 H5 0.9300 C5 C6 1.415(9) C6 C7 1.480(9) C7 C8 1.397(10) C7 C12 1.411(8) C8 H8 0.9300 C8 C9 1.374(10) C9 C10 1.376(10) C10 H10 0.9300 C10 C11 1.365(11) C11 C12 1.411(10) C13 H13A 0.9700 C13 H13B 0.9700 C13 C14 1.524(11) C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -2 945.59 24.2 0 0 2 968.52 22.23 0 0 3 1.54 2.27 0 0 3 1.93 1.23 0 0 -3 0.4 0.69 0 0 -3 1.31 0.91 0 0 4 352.75 18.97 0 0 -4 391.69 20.12 0 0 4 344.29 26.74 0 0 -4 351.2 20.58 0 0 5 7.36 3.29 0 0 5 -1.63 3.71 0 0 -5 3.22 2.76 0 0 -5 2.95 2.56 0 0 -6 16.39 5.41 0 0 6 15.46 4.84 0 0 -6 13.61 4.5 0 0 7 -1.66 10.46 0 0 -7 -0.57 0.87 0 0 7 3.04 2.18 0 0 7 0.25 1.47 0 0 -7 -2.6 3.79 0 0 -8 674.99 39.89 0 0 8 580.43 37.09 0 0 8 623.38 36.55 0 0 -8 616.56 38.95 0 0 9 -1.1 1.6 0 0 -9 -0.57 3.06 0 0 9 -0.05 2.07 0 0 -9 3.31 3.39 0 0 -9 2.06 3.2 0 0 -10 899.63 54 0 0 10 860.69 51.97 0 0 -10 870.43 49.53 0 0 10 956.11 50.81 0 0 11 0.81 1.36 0 0 -11 3.52 3.45 0 0 11 0.95 1.18 0 0 -12 177.82 27.74 0 0 -12 139.65 22 0 0 12 118.72 21.39 0 0 12 143.94 21.93 0 0 13 2.81 2.16 0 0 -13 -1.28 2.55 0 0 14 1411.49 81.92 0 0 -14 1623.15 81.19 0 0 15 -1.12 3.88 0 0 -15 0.27 2.91 0 0 -16 874.57 39.62 0 0 16 883.75 40.24 0 0 -17 0.53 1.86 0 0 17 -1.66 2.18 0 0 -18 14.96 5.04 0 0 18 13.22 4.6 0 0 19 0.42 1.1 0 0 -19 2.36 1.99 0 0 -20 11.21 4.17 0 0 20 8.49 3.9 0 0 21 -0.15 1.18 0 0 -21 0.83 1.06 0 0 22 430.23 23.04 0 0 23 1.76 1.78 0 0 24 69.09 6.98 0 1 0 1.29 1.16 0 -1 0 2.13 1.74 0 1 0 0.34 0.7 0 1 0 0.76 1.17 0 -1 -1 765.51 25.47 0 -1 1 768.94 29.25 0 1 -1 670.31 20.67 0 -1 -1 735.61 25.01 0 1 1 724.15 25.06 0 1 -1 784.25 21.85 0 1 1 773 21.98 0 1 -1 701.74 25.64 0 1 1 807.71 21.61 0 1 1 664.96 18.65 0 1 1 745.16 16.14 0 1 -1 728.82 22.88 0 -1 -2 551.38 24.66 0 1 2 513.95 20.65 0 1 2 493.46 15.95 0 1 2 582.41 21.25 0 1 -2 514.46 18.23 0 1 -2 492.94 21.68 0 -1 2 551.15 26.63 0 1 -2 529.58 22.18 0 1 2 502.83 17.76 0 1 -2 516.87 12.8 0 1 2 504.67 21.7 0 1 -2 523.58 20.61 0 -1 -2 481.5 15.47 0 1 -3 40.24 6.24 0 -1 3 40.2 6.92 0 1 3 36.49 5.24 0 -1 -3 40.19 4.9 0 1 -3 40.13 4.57 0 -1 3 42.41 7.95 0 -1 3 40.63 4.43 0 1 3 41.5 5.78 0 -1 -3 34.44 4.5 0 1 -3 39.49 6.69 0 1 3 50.22 6.37 0 1 -4 1801.33 53.79 0 -1 -4 1991.73 28.67 0 -1 4 1813.73 56.44 0 -1 4 1524.53 32.94 0 1 4 1766.69 42.33 0 1 4 1722.2 36.28 0 -1 4 1752.7 48.77 0 1 -4 1750.32 41.41 0 1 4 1733.37 43.16 0 -1 -4 1613.2 34.59 0 1 -4 1580.14 37.62 0 1 -5 733.59 39.69 0 1 5 668.22 30.61 0 -1 5 697.01 24.28 0 -1 -5 694.2 36.38 0 -1 5 680.41 32.67 0 1 5 659.78 30.13 0 -1 -5 583.43 22.8 0 1 -5 652.85 25.43 0 1 -5 705.51 20.78 0 1 5 727.93 36.34 0 1 5 643.2 21.61 0 -1 5 706.77 39.4 0 -1 6 2525.68 67.74 0 1 6 2445.46 72.12 0 1 -6 2577.1 83.87 0 -1 -6 2426.43 73.37 0 -1 6 2549.84 51.14 0 1 -6 2308.99 45.11 0 1 6 2230.47 64.72 0 -1 -6 2255.71 50.15 0 -1 6 2360.45 81.23 0 1 -6 2406.55 65.21 0 1 6 2310.2 63.5 0 -1 -7 1181.18 39.35 0 1 7 1196.5 50.17 0 -1 -7 1286.72 57.39 0 1 7 1005.3 49.91 0 1 7 1250.79 56.12 0 -1 7 1366.13 41.3 0 1 -7 1160.78 37.03 0 1 -7 1391.96 55.12 0 -1 7 1123.34 64.34 0 -1 7 1291.69 51.85 0 -1 8 1220.23 53.81 0 -1 8 1011.02 69.68 0 1 8 933.89 53.86 0 1 8 1196.02 58.36 0 -1 -8 1111.6 41.38 0 1 -8 1145.31 41.57 0 1 8 1154.64 53.94 0 -1 -8 1217.57 59.44 0 -1 9 1366.3 61.02 0 -1 -9 1334.19 66.44 0 1 9 1276.45 60.86 0 1 9 1208.51 66.14 0 1 9 1295.98 64.18 0 -1 -9 1259.69 47.75 0 1 10 0.14 2.53 0 -1 -10 2.75 2.9 0 1 10 2.34 4.52 0 -1 -10 -0.41 6.37 0 1 -10 1.06 1.72 0 -1 10 3.07 3.67 0 1 -10 17.76 14.51 0 -1 10 2.94 5.72 0 1 10 0.67 1.64 0 -1 -11 653.37 39.38 0 1 -11 1012.65 59.83 0 1 -11 709.3 64.56 0 1 11 813.62 60.17 0 1 11 664.44 50.27 0 -1 11 335.53 60.4 0 -1 -11 653.16 51.95 0 -1 11 721.19 50.05 0 -1 -12 81.44 19.44 0 -1 -12 70 15.31 0 -1 12 89.86 18.72 0 1 -12 113.95 21.03 0 1 -12 102.43 26.25 0 1 12 105.02 22.58 0 -1 -12 75.73 14.21 0 1 12 76.12 17.8 0 1 13 733.96 58.52 0 -1 -13 770.99 53.46 0 -1 13 816.25 59 0 -1 -13 840.4 64.4 0 -1 -13 789.21 49.22 0 1 -13 778.74 73.81 0 -1 14 97.35 21.28 0 1 -14 100.96 27.09 0 -1 -14 101.96 20.37 0 -1 -14 113.24 26.23 0 1 14 76.9 19.5 0 1 15 292.86 22.83 0 1 -15 316.18 24.32 0 -1 16 181.74 18.04 0 1 -16 236.57 21.22 0 1 16 201.58 19.27 0 1 -17 26.57 7.12 0 1 17 19.66 5.99 0 -1 17 18.43 5.5 0 -1 18 27.63 6.91 0 1 -18 30.81 7.77 0 1 18 28.46 7.07 0 -1 19 11.17 3.84 0 1 19 8.83 4.03 0 1 -19 7.74 3.32 0 1 -20 0.14 1.52 0 -1 20 3.03 2.57 0 1 20 1.9 1.86 0 -1 21 20.28 5.18 0 1 21 21.65 5.79 0 1 -21 23.58 5.76 0 -1 22 6.29 2.65 0 1 -22 6.74 3.03 0 1 22 5.32 2.5 0 -1 -23 143.3 10.95 0 -1 23 130.09 9.94 0 1 23 130.96 11.01 0 1 24 22.62 3.9 0 1 24 20.62 4.07 0 2 0 177.98 16 0 2 0 174.18 19.27 0 2 0 192.11 15.42 0 2 0 150.06 15.28 0 2 0 156.12 13.62 0 -2 0 174.66 14.99 0 -2 0 171.24 21.33 0 -2 -1 706.71 42.44 0 -2 1 743.86 45.86 0 2 1 674.24 34.44 0 2 1 755.33 30.65 0 -2 -1 668.86 32.31 0 2 -1 687.24 31.23 0 2 1 686.16 37.56 0 -2 1 716.74 26.25 0 2 -1 752.2 33.95 0 2 -1 854.81 34.74 0 2 1 737.6 31.73 0 2 -1 701.26 39.31 0 2 1 636.73 27.32 0 2 2 584.75 33.85 0 -2 -2 607.15 33.24 0 2 2 557.21 26.39 0 -2 -2 670.01 41.15 0 -2 -2 538.64 22.55 0 2 -2 653.23 33.6 0 2 -2 723.49 33.43 0 2 -2 627.78 37.63 0 2 -2 603.15 28.31 0 2 2 596.86 35.32 0 2 2 634.7 29.79 0 -2 2 625.72 44.43 0 -2 3 440.21 38.17 0 -2 -3 443.06 30.67 0 2 3 458.22 29.34 0 2 3 441.37 24.42 0 -2 -3 470.95 34.27 0 2 -3 476.86 30.7 0 2 3 496.52 28.4 0 2 3 429.98 32.39 0 2 -3 458.29 32.65 0 -2 -3 416.97 20.27 0 2 -3 523.27 30.08 0 2 -4 2981.58 83.96 0 -2 -4 2926.09 84.32 0 2 4 2560.55 86.17 0 -2 4 2901.67 103.74 0 2 -4 3075.19 83.74 0 2 4 2686.36 63.43 0 2 4 2959.61 59.53 0 -2 -4 2650.7 52.12 0 2 4 2948.08 72.77 0 2 -4 3200.78 80.89 0 2 5 168.37 15.79 0 -2 5 168.66 26.76 0 2 5 163.1 16.75 0 2 -5 168.1 20.11 0 2 -5 173.23 20.51 0 2 5 173.42 17.16 0 2 -5 176.14 21.8 0 -2 -5 177.89 22.11 0 -2 -5 164.48 13.5 0 2 5 143.07 22.12 0 2 6 1066.47 45.52 0 -2 -6 1033.13 35.56 0 2 -6 1268.01 61.57 0 2 6 1149.35 67.39 0 -2 6 1206.06 77.62 0 -2 -6 1234.57 62 0 2 -6 1193.25 61.62 0 2 6 1095.9 44.9 0 2 7 96.25 14.66 0 2 7 126.32 24.29 0 2 -7 120.72 20.85 0 2 -7 108.55 20.19 0 2 7 93.45 14.35 0 -2 7 93.25 22.96 0 -2 -7 98.84 11.66 0 -2 -7 115.99 20.01 0 -2 -8 209.86 18.1 0 2 -8 202.45 29.34 0 2 8 275.97 37.72 0 2 8 196.6 22.52 0 2 -8 207.56 30.51 0 -2 -8 233.73 30.19 0 -2 8 172.67 34.21 0 2 8 217.74 24.09 0 -2 -9 5.02 3.34 0 -2 -9 -0.41 5.86 0 2 9 4.72 4.44 0 2 -9 6.38 5.84 0 2 9 2.68 2.6 0 2 9 3.9 3.9 0 2 -9 1.63 4.28 0 -2 9 4.55 4.42 0 2 -10 811.03 69.77 0 2 10 834.62 53.26 0 -2 -10 951.77 43.22 0 2 10 826.64 54.82 0 2 -10 849.23 70.01 0 -2 10 658.94 80.07 0 -2 -10 907.24 65.93 0 -2 11 35.24 23.71 0 2 -11 37.89 16.13 0 2 11 28.84 10.17 0 2 11 72.69 21.48 0 2 11 30.14 10.33 0 2 -11 38.67 15.73 0 -2 -11 30.93 11.25 0 2 12 11.56 7.37 0 2 12 8.99 6.74 0 2 -12 6.28 3.18 0 2 12 2.13 2.41 0 2 -12 -0.08 4.37 0 -2 -12 -3.05 8.95 0 -2 -12 4.65 3.52 0 2 13 0.99 2.64 0 -2 -13 16.16 13.09 0 2 -13 -2 10.39 0 2 13 0.38 1.84 0 2 14 -2.14 3.02 0 2 -14 -0.48 1.66 0 2 15 124.33 14.98 0 2 -15 152.68 17.64 0 2 -16 78.66 12.65 0 2 16 71.92 11.42 0 2 17 21.16 6.11 0 2 -17 25.6 6.95 0 2 -18 210.91 19.54 0 2 18 180.92 17.61 0 2 19 20.79 5.67 0 2 -19 24.78 6.2 0 2 -20 258.65 19.29 0 2 20 253.29 18.56 0 2 21 76.52 10.67 0 2 -21 74.19 9.34 0 2 21 70.94 8.94 0 2 22 40.54 6.82 0 2 -22 34.83 5.67 0 2 22 37.73 5.67 0 -2 -23 23.76 4.02 0 2 23 20.78 4.11 0 3 0 -0.91 3.8 0 3 0 1.38 1.5 0 3 0 1.91 2.52 0 -3 0 0.4 3.78 0 -3 1 94.47 28.32 0 3 -1 106.21 16.6 0 3 1 110.97 21.19 0 3 -1 117.45 22.53 0 3 1 105.63 18 0 3 -1 108.81 17.51 0 3 1 102.6 16.2 0 -3 -1 53.24 21.46 0 3 -2 924.92 47.2 0 3 2 836.15 53.27 0 -3 2 850.88 86.46 0 3 -2 972.87 54.8 0 3 3 4.65 3.65 0 -3 3 3.98 6.52 0 3 3 9.35 5.39 0 3 -3 6.45 4.11 0 -3 -4 239.66 29.44 0 3 4 238.75 24.86 0 3 -4 294.25 33.33 0 3 4 227.86 31.55 0 -3 4 197.64 42.26 0 3 5 139.53 19.57 0 3 -5 161.96 26.17 0 -3 5 118.51 34.35 0 -3 -5 139.5 23.85 0 3 5 134.76 25.51 0 3 6 46 11.65 0 3 6 32.82 13.58 0 3 -6 56.8 16.11 0 -3 6 36.02 21.16 0 -3 -6 49.05 15.46 0 -3 -7 180.04 30.26 0 3 7 180.04 33.33 0 3 7 184.17 24.66 0 -3 7 158.09 44.82 0 3 -7 202.48 32.97 0 3 8 172.4 34.02 0 3 -8 144.38 29.33 0 -3 -8 185.28 31.98 0 3 8 169.28 24.65 0 -3 8 134.11 42.96 0 3 9 68.26 22 0 3 9 39.63 12.1 0 -3 9 17.84 12.68 0 -3 -9 42.09 14.77 0 3 -9 37.46 16.42 0 3 10 144.83 16.67 0 3 11 47.08 9.69 0 3 12 507.79 31.51 0 3 13 67.11 11.39 0 3 14 248.91 21.08 0 3 14 118.55 17.08 0 3 15 11.89 4.88 0 3 -15 15.43 5.25 0 3 -16 2.13 1.44 0 3 16 1.03 1.21 0 3 -17 2.51 2.33 0 3 17 1.32 2.1 0 3 -18 5.52 2.91 0 3 18 4.87 3.06 0 3 19 22 5.75 0 3 -19 22.92 4.53 0 3 -19 17.3 4.68 0 3 20 38.84 6.57 0 -3 -21 6.69 2.19 0 4 0 514.84 27.67 0 4 0 636.92 42.55 0 4 -1 314.94 30.19 0 4 1 304.41 28.72 0 4 -1 273.41 19.73 0 4 1 249.08 19.77 0 4 -2 19.85 7.58 0 4 -2 10.09 3.38 0 4 2 14.55 6.12 0 4 2 19.18 6.75 0 4 3 7.27 2.71 0 4 -3 11.22 5.62 0 4 -3 4.62 1.97 0 4 3 11.15 5.27 0 4 -4 49.98 9.21 0 4 -4 64.57 13.51 0 4 4 73.73 12.59 0 4 4 54.97 9.74 0 4 -5 103.87 13.85 0 4 5 124.45 14.99 0 4 -5 171.29 22.11 0 4 5 170.98 18.54 0 4 6 142.01 16.3 0 4 -6 75.33 12.06 0 4 -6 160.56 20.78 0 4 6 64.92 9.98 0 4 7 103.08 12.02 0 4 7 165.06 16.95 0 4 8 10.17 4.96 0 4 9 -1.65 7.29 0 4 10 16.18 4.6 0 4 11 -6.84 3.97 0 4 12 47.18 8.47 0 4 -13 6.87 3.31 0 4 13 20.75 7.33 0 4 14 98.47 13.64 0 4 -14 57.31 10.3 0 4 15 79.59 11.71 0 4 -15 36.77 7.79 0 4 -16 34.31 6.87 0 4 -17 7.46 2.67 0 4 -18 0.25 0.73 0 5 0 5.15 2.01 0 5 1 3.49 4.91 0 5 -1 2.03 1.9 0 5 2 8.4 5.34 0 5 -2 7.75 3.55 0 5 3 -8.35 5.25 0 5 -3 -1.32 4.66 0 5 -4 29.87 10.19 0 5 4 37.83 9.92 0 5 -4 26.56 7.27 0 5 -5 4.89 3.95 0 5 5 2.28 2.81 0 5 6 375.88 31.19 0 5 6 209.25 21.37 0 5 -6 102.71 14.73 0 5 -6 270.17 29.3 0 5 -7 6.8 4.21 0 5 7 5.59 3.46 0 5 8 387.05 31.84 0 5 -8 122.38 16.17 0 5 -9 4.21 3.01 0 5 9 205.1 23.9 0 5 10 181.81 22.77 0 5 -10 1.18 0.85 0 5 -11 0.77 0.78 0 5 -12 0.06 1.15 0 5 -13 22.66 5.71 0 5 -14 25.96 5.36 0 6 0 125.86 21.5 0 6 1 -21.67 9.94 0 6 -2 -24.84 16.31 0 6 2 -36.79 11.92 0 6 3 -26.05 9.25 0 6 -3 -38.24 13.17 0 6 4 -9.62 6.78 0 6 -4 -15.02 10.96 -1 0 24 17.92 3.59 -1 0 23 0.56 1.23 -1 0 22 3.25 2.08 1 0 -22 4.62 1.9 1 0 -21 0.84 1.34 -1 0 21 0.1 0.87 1 0 -20 426.64 25.71 -1 0 20 431.8 26.66 -1 0 19 1.44 2.63 1 0 -19 2.1 2.5 -1 0 18 7.47 3.35 1 0 -18 5.35 3.29 -1 0 17 -0.63 0.73 1 0 -17 1.17 1.64 -1 0 16 186.57 18.42 1 0 -16 188.26 18.26 1 0 -15 -0.28 2.04 -1 0 15 3.46 5.75 1 0 -14 1428.69 75.78 -1 0 14 1243.4 76.82 1 0 -13 0.49 3.52 1 0 -13 15.57 12.99 -1 0 13 1.44 3.71 -1 0 13 2.12 5.01 -1 0 12 1890.82 82.33 -1 0 12 1733.77 82.84 1 0 -12 1921 86.05 -1 0 11 -0.05 2.61 1 0 -11 -1.42 3.92 1 0 -11 2.07 3.11 -1 0 11 1.47 1.15 -1 0 10 336.73 32.65 1 0 -10 379.5 33.76 -1 0 10 419.59 35.26 1 0 -10 413.03 35.15 -1 0 9 1.81 2.92 -1 0 9 4.47 4.79 1 0 -9 0.99 2.04 -1 0 8 56.71 11.98 -1 0 8 57.41 11.48 1 0 -8 57.11 11.71 1 0 -8 55.95 10.95 1 0 -7 0.83 1.25 -1 0 7 0.96 1.59 -1 0 7 5.06 3.63 1 0 -7 2.64 3.48 1 0 -6 5203.54 97.64 1 0 -6 5283.77 89.57 1 0 -5 0.09 1.26 -1 0 5 3.36 2.28 1 0 -5 -1.66 2.34 1 0 -4 5302.77 82.53 1 0 -4 5507.54 71 1 0 -3 1.55 1.1 -1 0 3 8.09 3.32 1 0 -2 793.85 24.51 1 0 -2 680.88 21.75 1 0 -1 0.65 0.5 -1 0 -1 0.51 0.43 -1 0 -1 5.02 1.33 -1 0 -2 58.62 5.79 -1 0 -2 61.1 6.28 -1 0 -3 0.24 1.09 -1 0 -3 -0.02 0.56 1 0 3 0.64 0.47 -1 0 -4 82.51 10.02 1 0 4 94.13 7.19 1 0 4 87.71 8.62 -1 0 -4 82.58 9.9 -1 0 -5 7.23 3.23 1 0 5 1.26 1.42 -1 0 -5 6.79 3.71 1 0 5 1.57 1.31 1 0 6 3.82 2.66 -1 0 -6 5.95 3.87 1 0 6 5.22 3.36 1 0 6 4.44 2.64 -1 0 -6 4.66 3.75 1 0 7 3.66 5.39 -1 0 -7 1.16 3.26 -1 0 -7 1.09 2.15 1 0 7 0.24 1.45 1 0 7 -0.32 1.51 1 0 8 2310.32 73.03 -1 0 -8 2301.01 77.12 1 0 8 2413.73 68.01 -1 0 -9 -0.05 2.27 1 0 9 0.05 1.4 -1 0 -9 8.16 8.04 1 0 9 -0.54 2.91 -1 0 -10 3982.21 114.48 1 0 10 3919.75 109.81 -1 0 -11 1.22 3.29 1 0 11 -1.57 2.75 -1 0 -11 -1.02 2.39 -1 0 -12 1260.76 71.11 1 0 12 1201.61 68.4 -1 0 -12 1260.72 65.25 1 0 13 -0.52 2.41 -1 0 -13 1.78 2.75 -1 0 -14 7.86 12.35 -1 0 -14 2.6 4.08 1 0 14 1.45 1.64 -1 0 -15 -3.11 1.95 -1 0 -15 10.38 10.34 -1 0 -16 228.56 20.22 1 0 16 242.38 20.92 1 0 17 1.5 1.69 -1 0 -17 -1.2 1.49 -1 0 -18 356.21 25.33 1 0 18 357.07 25.61 1 0 19 -0.11 1.92 -1 0 -19 2.49 1.93 -1 0 -20 5.09 2.6 1 0 20 3.91 2.63 -1 0 -21 3.23 2.5 1 0 21 1.4 1.78 -1 0 -21 0.57 1.21 1 0 22 7.36 2.99 1 0 23 -1.02 1.2 1 0 24 166.93 10.99 -1 1 24 4.46 1.81 -1 1 23 86.24 9.01 1 1 -23 78.01 8.4 -1 -1 23 94.46 8.63 -1 1 22 45.89 7.41 1 1 -22 44.05 7.14 -1 -1 22 52.45 7.34 -1 1 21 79.22 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0 12.54 4.9 -12 1 -1 540.2 36.83 -12 -1 -1 455.72 28.41 12 1 1 544.41 30.91 -12 1 -2 115.12 17.32 -12 -1 -2 110.49 13.98 -12 1 -3 101.31 16.44 -12 -1 -3 101.3 13.7 -12 1 -4 55.59 12.19 -12 -1 -4 49.97 9.74 -12 -1 -5 45.68 9.46 -12 1 -5 44.81 11.14 -12 1 -6 285.36 28.73 -12 -1 -6 235.91 22.08 -12 1 -7 125.26 19.08 -12 -1 -7 109.31 15.12 -12 1 -8 333.15 31.12 -12 -1 -8 290.1 25.18 -12 1 -9 27.68 9.15 -12 -1 -9 29.17 8.02 -12 1 -10 17.33 6.6 -12 -1 -10 18.54 6.73 -12 1 -11 1.74 1.46 -12 -1 -11 0.41 1.82 -12 1 -12 64.19 12.74 -12 -1 -12 60.58 11.08 -12 1 -13 4.31 3.32 -12 -1 -13 0.93 1.64 -12 1 -14 5.79 3.01 -12 -1 -14 2.7 2.62 -12 -1 -15 14.57 4.46 -12 -1 -16 27.71 5.42 -12 2 19 4.56 1.68 12 2 -19 4.81 1.9 -12 2 18 17.41 3.94 12 2 -18 20.5 4.45 -12 2 17 15.6 4.07 12 2 -17 9.86 3.05 -12 2 16 24.68 5.82 12 2 -16 19.33 5.12 -12 2 15 8.51 3.82 12 2 -15 8.19 3.72 -12 2 14 218.6 20.32 12 2 -14 183.38 17.97 -12 2 13 104.55 14.88 12 2 -13 81.36 12.37 -12 2 12 62.78 12 12 2 -12 51.96 10.34 -12 2 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