#------------------------------------------------------------------------------ #$Date: 2021-07-14 02:51:34 +0300 (Wed, 14 Jul 2021) $ #$Revision: 267518 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/41/1564145.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_1564145 loop_ _publ_author_name 'Bai, Tianwen' 'Zhou, Peng' 'Li, Zixian' 'Zheng, Botuo' 'Ling, Jun' _publ_section_title ; Seeding Crystals, Harvesting Polypeptides: Preparing Long Chiral-Sequence Controlled Polypeptides by Interlocked Polymerization in Cocrystals (iPiC) of N-Thiocarboxyanhydride (NTA) at Room Temperature ; _journal_name_full Macromolecules _journal_paper_doi 10.1021/acs.macromol.1c00371 _journal_year 2021 _chemical_formula_moiety 'C6 H9 N O2 S2' _chemical_formula_sum 'C6 H9 N O2 S2' _chemical_formula_weight 191.26 _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 direct _audit_creation_date 2016-12-30 _audit_creation_method ; Olex2 1.2 (compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269) ; _cell_angle_alpha 90 _cell_angle_beta 101.719(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.1451(16) _cell_length_b 7.7606(7) _cell_length_c 9.2513(10) _cell_measurement_reflns_used 1239 _cell_measurement_temperature 170.9 _cell_measurement_theta_max 29.4032 _cell_measurement_theta_min 3.1281 _cell_volume 853.79(17) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 170.9 _diffrn_detector_area_resol_mean 10.3592 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -21.00 82.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 10.8433 77.0000 90.0000 103 #__ type_ start__ end____ width___ exp.time_ 2 omega -21.00 49.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -12.7183 38.0000 -30.0000 70 ; _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0329318000 _diffrn_orient_matrix_UB_12 0.0564116000 _diffrn_orient_matrix_UB_13 -0.0339946000 _diffrn_orient_matrix_UB_21 -0.0258829000 _diffrn_orient_matrix_UB_22 0.0720184000 _diffrn_orient_matrix_UB_23 0.0267398000 _diffrn_orient_matrix_UB_31 0.0423964000 _diffrn_orient_matrix_UB_32 -0.0000457000 _diffrn_orient_matrix_UB_33 0.0653013000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 3132 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.347 _diffrn_reflns_theta_min 3.134 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.573 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.488 _exptl_crystal_description block _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.4 _refine_diff_density_max 1.231 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 101 _refine_ls_number_reflns 1563 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0569 _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^)+(0.0490P)^2^+1.8685P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1284 _refine_ls_wR_factor_ref 0.1383 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1296 _reflns_number_total 1563 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ma1c00371_si_002.cif _cod_data_source_block 161229_sc_metdl _cod_original_cell_volume 853.78(17) _cod_database_code 1564145 _chemical_oxdiff_formula 'c10 h10 n2 o8 S1' _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 0.803 _shelx_estimated_absorpt_t_min 0.770 _reflns_odcompleteness_completeness 99.57 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C3(H3) 2.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B) 2.c Aromatic/amide H refined with riding coordinates: N1(H1) 2.d Idealised Me refined as rotating group: C6(H6A,H6B,H6C) ; _shelx_res_file ; TITL 161229_SC_MeTDL in P21/c #14 161229_sc_metdl.res created by SHELXL-2016/6 at 14:15:54 on 30-Dec-2016 REM reset to P21/c #14 CELL 0.71073 12.14505 7.76055 9.25127 90 101.7188 90 ZERR 4 0.00164 0.00074 0.001 0 0.0113 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 24 36 4 8 8 L.S. 4 PLAN 20 SIZE 0.48 0.42 0.4 TEMP -103.15 BOND $H htab fmap 2 acta SHEL 999 0.83 REM REM REM WGHT 0.049000 1.868500 FVAR 7.54005 S1 5 0.894614 0.099315 0.660505 11.00000 0.03788 0.02510 = 0.04878 0.00924 0.01877 0.00222 S2 5 0.637694 0.758012 0.514782 11.00000 0.08371 0.04793 = 0.03668 0.00450 0.02053 0.00550 O2 4 1.039504 0.278701 0.544898 11.00000 0.03153 0.03251 = 0.05694 0.01145 0.02387 0.00670 O1 4 0.700117 0.155451 0.737284 11.00000 0.04018 0.03840 = 0.06317 0.00963 0.02881 -0.00572 N1 3 0.877961 0.413223 0.569092 11.00000 0.02814 0.02377 = 0.04892 0.00977 0.01984 0.00183 AFIX 43 H1 2 0.895520 0.512229 0.533265 11.00000 -1.20000 AFIX 0 C3 1 0.771102 0.393988 0.615057 11.00000 0.02998 0.03158 = 0.03723 0.00454 0.01454 -0.00018 AFIX 13 H3 2 0.708487 0.402838 0.526593 11.00000 -1.20000 AFIX 0 C2 1 0.948876 0.282216 0.581001 11.00000 0.03134 0.02643 = 0.02800 0.00285 0.00771 0.00037 C1 1 0.771970 0.213991 0.679897 11.00000 0.03326 0.02982 = 0.03714 0.00002 0.01068 -0.00378 C4 1 0.753813 0.526271 0.727687 11.00000 0.03523 0.03642 = 0.03460 -0.00120 0.01173 -0.00312 AFIX 23 H4A 2 0.815833 0.516961 0.815182 11.00000 -1.20000 H4B 2 0.682599 0.500960 0.759895 11.00000 -1.20000 AFIX 0 C5 1 0.749600 0.710607 0.668470 11.00000 0.04101 0.02920 = 0.06117 -0.00123 0.02926 -0.00096 AFIX 23 H5A 2 0.821906 0.735326 0.638935 11.00000 -1.20000 H5B 2 0.743379 0.790242 0.750028 11.00000 -1.20000 AFIX 0 C6 1 0.521005 0.780873 0.606408 11.00000 0.03677 0.08347 = 0.06643 0.02103 0.00072 -0.00482 AFIX 137 H6A 2 0.454042 0.816835 0.534679 11.00000 -1.50000 H6B 2 0.539135 0.867947 0.684339 11.00000 -1.50000 H6C 2 0.506370 0.670273 0.650042 11.00000 -1.50000 AFIX 0 HKLF 4 REM 161229_SC_MeTDL in P21/c #14 REM R1 = 0.0569 for 1296 Fo > 4sig(Fo) and 0.0689 for all 1563 data REM 101 parameters refined using 0 restraints END WGHT 0.0488 1.8736 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+1, -z+1 HTAB N1 O2_$1 EQIV $2 x, y+1, z HTAB C5 S1_$2 HTAB C5 O2_$1 EQIV $3 x, -y+3/2, z+1/2 HTAB C5 S2_$3 REM Highest difference peak 1.231, deepest hole -0.531, 1-sigma level 0.078 Q1 1 0.5795 0.8315 0.4799 11.00000 0.05 1.23 Q2 1 0.7000 0.5116 0.6081 11.00000 0.05 0.69 Q3 1 0.8140 0.4208 0.7137 11.00000 0.05 0.60 Q4 1 0.7158 0.6875 0.5833 11.00000 0.05 0.42 Q5 1 0.7722 0.3093 0.6398 11.00000 0.05 0.24 Q6 1 0.9181 0.1882 0.6006 11.00000 0.05 0.23 Q7 1 0.9437 0.4990 0.6545 11.00000 0.05 0.22 Q8 1 0.9058 0.4119 0.6625 11.00000 0.05 0.22 Q9 1 0.5949 0.6607 0.4953 11.00000 0.05 0.21 Q10 1 0.5170 0.6084 0.6032 11.00000 0.05 0.21 Q11 1 0.8211 0.3979 0.5750 11.00000 0.05 0.21 Q12 1 0.6749 0.6062 0.5279 11.00000 0.05 0.20 Q13 1 0.9411 0.3591 0.6287 11.00000 0.05 0.20 Q14 1 0.7931 0.2454 0.7457 11.00000 0.05 0.19 Q15 1 1.1073 0.3428 0.5781 11.00000 0.05 0.19 Q16 1 0.6810 0.8283 0.4580 11.00000 0.05 0.19 Q17 1 0.7703 0.6284 0.6759 11.00000 0.05 0.19 Q18 1 0.8264 0.1542 0.6565 11.00000 0.05 0.18 Q19 1 0.9791 0.2172 0.4734 11.00000 0.05 0.18 Q20 1 0.7512 0.2553 0.8187 11.00000 0.05 0.18 ; _shelx_res_checksum 51332 _shelx_hkl_file ; 3 0 0 18287.8 692.863 2 -4 0 0 219.283 103.606 2 4 0 0 76.6130 71.8168 2 -5 0 0 147022. 2541.83 2 5 0 0 144229. 2495.02 2 6 0 0 67565.4 1871.46 2 7 0 0 56210.4 1847.90 2 8 0 0 72302.6 2277.55 2 9 0 0 28125.7 1519.55 2 10 0 0 51.7264 198.830 2 11 0 0 2733.17 548.472 2 12 0 0 9538.46 1062.68 2 13 0 0 2744.18 595.575 2 14 0 0 10498.4 1227.01 2 15 0 0 10715.3 1275.92 2 16 0 0 28.4795 200.220 2 -1 1 0 8094.66 326.461 1 2 -1 0 459748. 3326.03 2 -2 1 0 460286. 3109.08 1 3 -1 0 14466.4 692.991 2 4 -1 0 8204.64 581.379 2 -5 1 0 3352.57 422.431 2 5 1 0 3184.93 364.516 2 5 -1 0 2822.17 382.460 2 6 -1 0 108967. 2534.46 2 6 1 0 111502. 2375.19 2 -6 1 0 114896. 2665.80 2 7 1 0 25087.6 1251.78 2 7 -1 0 24781.2 1295.17 2 -8 1 0 4065.84 572.920 2 8 -1 0 4474.23 595.768 2 8 1 0 4839.64 592.584 2 -9 1 0 68295.0 2476.68 2 9 -1 0 61292.6 2335.83 2 9 1 0 63413.8 2247.83 2 10 -1 0 21078.0 1451.28 2 10 1 0 20390.4 1353.40 2 11 -1 0 8325.05 964.105 2 11 1 0 6745.11 829.771 2 12 -1 0 899.049 375.096 2 12 1 0 1054.57 417.449 2 13 1 0 442.871 295.512 2 13 -1 0 510.092 264.100 2 14 -1 0 1096.62 407.257 2 14 1 0 1362.51 467.726 2 15 1 0 834.493 411.605 2 15 -1 0 645.131 369.246 2 16 1 0 802.559 388.498 2 0 2 0 550545. 3208.61 1 -1 2 0 63676.3 1133.74 1 1 2 0 63103.5 1220.40 1 -2 2 0 27896.6 843.506 1 2 -2 0 27048.4 985.989 2 2 -2 0 27592.6 847.473 1 -3 2 0 177761. 2428.66 1 3 -2 0 179809. 2786.03 2 -4 2 0 30074.6 1126.00 1 4 -2 0 31912.5 1259.14 2 -5 2 0 32720.6 1301.22 1 5 -2 0 32995.4 1362.46 2 6 -2 0 17949.1 1088.94 2 -6 2 0 17389.7 1060.01 1 7 -2 0 47901.2 1892.91 2 7 2 0 49953.8 1732.27 2 8 2 0 165.291 132.597 2 8 -2 0 568.777 244.923 2 -8 2 0 606.840 257.127 2 9 2 0 20224.4 1279.14 2 9 -2 0 20102.5 1385.64 2 10 2 0 23514.6 1449.61 2 10 -2 0 24727.6 1608.79 2 11 2 0 1590.89 436.766 2 11 -2 0 2120.61 510.777 2 12 -2 0 3811.32 722.734 2 12 2 0 3709.07 644.199 2 13 -2 0 180.861 244.449 2 13 2 0-29.2840 196.959 2 14 2 0 574.785 320.702 2 14 -2 0 1074.45 454.704 2 15 2 0-267.744 237.105 2 15 -2 0 445.348 385.032 2 0 -3 0-96.0811 98.0665 1 0 3 0 8.94869 88.3270 1 1 3 0 369492. 3434.77 1 1 -3 0 366373. 3288.14 1 -1 -3 0 369026. 3358.77 1 -1 3 0 370881. 3218.77 1 -2 3 0 17728.8 755.616 1 -2 -3 0 16478.2 770.075 1 2 -3 0 18266.5 781.257 1 -3 -3 0 175383. 2792.55 1 3 -3 0 178409. 2658.10 1 -3 3 0 178077. 2607.14 1 3 -3 0 176079. 3161.33 2 4 -3 0 41152.2 1594.56 2 -4 3 0 43208.6 1437.91 1 5 -3 0 32759.6 1512.29 2 -5 3 0 32284.5 1346.61 1 -6 3 0 11444.8 868.365 1 6 -3 0 10348.1 902.231 2 -7 3 0 39568.0 1713.29 1 -7 3 0 41798.0 1906.63 2 7 -3 0 39863.6 1865.44 2 -8 3 0 22330.6 1394.91 1 8 -3 0 31306.5 1735.52 2 9 -3 0 10907.1 1080.39 2 9 3 0 12736.9 1023.69 2 10 3 0 838.671 304.576 2 10 -3 0 1532.06 457.004 2 11 3 0 21306.9 1491.21 2 11 -3 0 23262.7 1718.04 2 12 3 0 16788.1 1376.55 2 12 -3 0 18123.7 1598.71 2 13 3 0 1659.73 440.018 2 13 -3 0 2067.18 553.052 2 14 3 0-588.369 295.577 2 14 -3 0-204.724 290.962 2 15 3 0 282.909 264.507 2 0 4 0 27195.9 1009.88 1 0 -4 0 27301.3 1020.00 1 -1 4 0 42748.6 1270.25 1 1 -4 0 40748.7 1249.08 1 -1 -4 0 40369.7 1268.43 1 1 4 0 42964.3 1341.14 1 -2 4 0 992.842 209.172 1 2 -4 0 1442.37 254.210 1 -2 -4 0 1249.86 257.718 1 3 -4 0 74250.5 1872.79 1 -3 -4 0 74409.2 1944.26 1 -3 4 0 78736.2 1876.63 1 -4 4 0 25314.2 1144.78 1 5 -4 0 83861.5 2664.12 2 -5 4 0 87568.2 2263.82 1 6 -4 0 14073.8 1142.25 2 -6 4 0 15185.3 1029.65 1 -6 -4 0 14775.6 1094.39 1 -7 4 0 23298.2 1364.51 1 7 -4 0 29405.5 1708.49 2 -8 4 0 393.010 245.646 1 8 -4 0 20.5570 234.284 2 9 -4 0 21508.2 1610.08 2 10 4 0 54240.5 2285.39 2 10 -4 0 55331.9 2692.54 2 11 -4 0 500.964 309.034 2 11 4 0 567.325 255.935 2 12 -4 0 530.135 349.052 2 12 4 0-89.9532 122.612 2 13 4 0-398.774 242.115 2 13 -4 0 205.079 209.013 2 14 4 0 198.123 283.289 2 0 -5 0 1343.85 365.444 1 0 5 0 287.436 211.673 1 1 5 0 59720.8 1783.77 1 1 -5 0 55307.4 1648.36 1 -1 5 0 57091.1 1640.99 1 -1 -5 0 61232.3 1752.14 1 -1 5 0 56305.0 2024.43 2 -2 5 0 53614.0 2061.71 2 -2 5 0 56247.2 1674.29 1 2 -5 0 52810.4 1658.83 1 3 -5 0 217.043 152.002 1 -3 5 0 522.931 256.049 2 -3 5 0 393.454 172.748 1 -4 5 0 12115.9 844.515 1 -5 -5 0 1336.58 330.687 1 -5 5 0 1035.60 263.922 1 -6 -5 0 3968.21 601.454 1 -6 5 0 3461.68 513.289 1 -7 5 0 738.208 252.678 1 -7 -5 0 567.512 152.297 1 7 -5 0 664.716 313.871 2 -8 -5 0 267.970 206.795 1 8 -5 0 420.055 233.449 2 9 -5 0 5643.94 880.639 2 -9 -5 0 5958.61 860.660 1 10 -5 0 2543.54 616.525 2 -10 -5 0 2173.44 541.435 1 11 -5 0-115.061 141.409 2 11 5 0 94.0165 125.343 2 -11 -5 0 2.52611 258.927 1 12 5 0 468.249 289.190 2 12 -5 0 854.149 427.015 2 -12 -5 0 171.340 241.140 1 -13 -5 0 442.531 367.719 1 13 -5 0-84.5152 164.494 2 13 5 0 488.554 283.413 2 0 6 0 120470. 3196.75 2 0 6 0 84733.8 2258.02 1 -1 6 0 15894.7 974.719 1 1 6 0 13494.9 934.026 1 -2 6 0 4877.01 543.496 1 -3 -6 0 471.815 164.207 1 -3 6 0 358.942 161.247 1 -4 -6 0 55990.2 2068.77 1 -4 6 0 56591.4 1925.98 1 -5 6 0 2509.19 426.269 1 -5 -6 0 2802.09 480.320 1 -6 -6 0 2060.35 437.859 1 -6 6 0 1628.86 363.856 1 -7 -6 0 12200.2 1145.03 1 -8 -6 0 22774.1 1630.71 1 -9 -6 0 12589.7 1265.59 1 -10 -6 0 69.8758 148.281 1 -11 -6 0 1855.75 545.520 1 -12 -6 0 1714.30 566.525 1 0 -7 0-172.485 178.787 1 0 7 0-446.578 196.597 1 -1 7 0 5115.22 586.796 1 -1 -7 0 6293.36 683.788 1 -2 -7 0 77332.8 2410.65 1 -2 7 0 78780.0 2316.39 1 -3 7 0 1781.96 359.673 1 -3 -7 0 2182.53 421.479 1 3 -7 0 1617.04 354.605 1 4 -7 0 156.224 136.890 1 -4 -7 0-4.32429 108.228 1 -4 7 0 85.4579 159.270 1 -5 7 0 6657.41 713.998 1 -5 -7 0 7040.71 831.662 1 -6 -7 0 17856.5 1360.16 1 -7 -7 0 27781.6 1766.48 1 -8 -7 0 4770.29 768.762 1 -9 -7 0 1547.89 458.915 1 -10 -7 0 5460.35 898.493 1 -11 -7 0 467.312 298.431 1 0 -8 0 12733.1 1015.73 1 -1 -8 0 429.337 191.197 1 1 -8 0 598.429 250.001 1 2 -8 0-33.4690 134.226 1 -2 -8 0 248.532 214.595 1 -3 -8 0 4068.70 622.659 1 3 -8 0 2674.62 486.969 1 -4 -8 0 4723.73 678.207 1 4 -8 0 3556.98 564.604 1 -5 -8 0-107.759 140.156 1 -6 -8 0-244.760 200.210 1 -7 -8 0 3659.04 668.074 1 -8 -8 0 723.525 315.433 1 -9 -8 0-127.801 161.600 1 -10 -8 0-33.0090 338.763 1 0 -9 0-282.635 243.824 1 -1 -9 0 13224.4 1119.65 1 -2 -9 0 2468.73 489.066 1 -3 -9 0 5683.10 770.302 1 -4 -9 0 674.388 275.746 1 -5 -9 0 1975.03 454.216 1 -6 -9 0-105.148 146.697 1 -7 -9 0 7451.10 1016.31 1 -8 -9 0 4480.63 785.258 1 16 0 -1 605.939 437.353 2 15 0 -1 103.860 147.707 2 14 0 -1 269.118 217.750 2 13 0 -1 326.454 241.171 2 12 0 -1 484.376 285.082 2 11 0 -1 183.663 265.321 2 10 0 -1-67.7079 183.026 2 9 0 -1-35.6589 150.752 2 8 0 -1 73.6383 120.432 2 7 0 -1 51.6090 88.8097 2 6 0 -1-17.3595 107.888 2 5 0 -1 99.0751 98.9319 2 4 0 -1 38.8935 75.1082 2 3 0 -1 141.715 84.9357 2 -2 0 1 208.930 72.3230 1 -2 0 -1 172.740 71.9002 2 2 0 1 128.025 53.7354 2 3 0 1 111.936 78.0866 2 -3 0 -1 68.5949 70.3738 2 4 0 1 12.7944 59.1530 2 -4 0 -1 53.6141 63.0165 2 -5 0 -1 47.9465 75.0227 2 5 0 1-37.6632 70.6196 2 6 0 1 50.1170 94.7242 2 -6 0 -1 157.598 119.455 2 -7 0 -1 195.132 168.616 2 7 0 1-135.868 150.635 2 8 0 1 241.129 196.888 2 9 0 1-139.044 205.014 2 10 0 1 87.4109 135.507 2 11 0 1 1033.44 461.350 2 12 0 1 808.135 405.240 2 13 0 1-98.1610 306.204 2 14 0 1 87.4238 104.877 2 15 0 1 622.067 383.695 2 16 0 1 436.199 329.104 2 16 1 -1 117.548 236.665 2 15 1 -1-354.021 259.044 2 15 -1 -1 361.011 246.436 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558.088 237.619 2 9 1 4 361.437 168.917 2 -9 -1 -4 332.983 227.280 1 10 1 4 2139.49 383.705 2 -10 -1 -4 2447.22 597.977 1 -11 -1 -4 7244.62 1081.33 1 11 1 4 5751.49 667.936 2 -12 -1 -4 654.348 408.012 1 -13 -1 -4 2999.91 789.293 1 15 2 -4 2249.25 672.486 2 14 2 -4 822.599 402.192 2 14 -2 -4 1628.45 535.429 2 13 2 -4 665.498 354.117 2 13 -2 -4 73.5644 182.229 2 12 -2 -4 12899.7 1367.93 2 12 2 -4 10934.0 1239.76 2 11 2 -4 3896.45 715.297 2 11 -2 -4 3536.69 696.539 2 10 -2 -4 14189.0 1301.46 2 10 2 -4 13447.0 1253.10 2 9 -2 -4 2857.92 560.541 2 8 -2 -4 12419.6 1099.79 2 -8 -2 4 13763.4 1106.04 1 7 -2 -4 1687.99 405.143 2 -7 -2 4 2050.66 387.349 1 -7 2 4 1653.02 453.994 1 -6 2 4 10095.7 907.136 1 6 -2 -4 9479.65 852.552 2 -6 -2 4 9597.57 777.007 1 -5 2 4 20721.0 1239.29 1 5 -2 -4 22430.7 1209.44 2 -5 -2 4 21542.8 1059.04 1 4 -2 -4 128540. 2680.33 2 -4 2 4 129339. 2957.73 1 -4 -2 4 130441. 2348.29 1 -3 -2 4 15034.3 707.871 1 3 -2 -4 13700.5 799.984 2 -3 2 4 13924.6 943.278 1 -2 -2 4 13381.8 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1132.82 2 9 -3 -8 8138.45 1174.64 1 8 -3 -8 1709.11 449.202 2 8 -3 -8 2161.20 584.064 1 7 -3 -8 2736.91 549.032 2 7 -3 -8 2606.58 627.071 1 -6 -3 8 3625.22 507.670 1 6 -3 -8 3570.46 596.573 2 6 -3 -8 4076.41 742.182 1 5 -3 -8 10112.4 942.305 2 -5 -3 8 11097.1 814.574 1 5 -3 -8 10215.1 1159.82 1 4 -3 -8 28104.6 1879.73 1 4 -3 -8 28920.1 1490.75 2 -4 -3 8 30973.3 1256.57 1 3 -3 -8-81.8073 295.456 1 3 -3 -8 363.419 183.413 2 -3 -3 8 233.299 95.4991 1 2 -3 -8 15201.2 1351.66 1 2 -3 -8 15516.9 893.109 2 -2 -3 8 12062.1 688.506 1 1 -3 -8 9060.33 1041.96 1 1 -3 -8 9185.22 565.210 2 1 3 -8 9457.03 611.160 1 0 -3 -8 19726.4 1557.77 1 0 3 -8 22614.0 934.034 1 -1 3 -8 637.332 179.170 1 -1 -3 -8 207.765 213.316 1 -2 3 -8 10377.3 684.733 1 -2 -3 -8 9286.37 1084.47 1 -3 3 -8 2477.39 381.428 1 -3 -3 -8 2321.04 541.465 1 -4 3 -8 12687.8 868.766 1 -4 -3 -8 11092.6 1261.79 1 -5 -3 -8 834.374 406.655 1 -6 -3 -8 10598.6 1292.12 1 -7 -3 -8 947.493 360.094 1 -8 -3 -8 4414.71 875.787 1 12 -4 -8 1666.24 579.644 2 11 -4 -8 9671.73 1246.86 2 10 -4 -8 1299.25 448.557 2 9 -4 -8 101.385 209.870 2 9 -4 -8-379.935 318.032 1 8 -4 -8 5467.39 832.974 2 8 -4 -8 4876.26 907.068 1 7 -4 -8 2139.97 484.477 2 7 -4 -8 3009.37 740.770 1 6 -4 -8 1796.70 443.012 2 6 -4 -8 1853.47 559.590 1 5 -4 -8 2611.35 651.488 1 5 -4 -8 2691.02 480.969 2 4 -4 -8 12974.3 1353.93 1 4 -4 -8 12124.6 953.999 2 3 -4 -8 10950.2 1229.27 1 3 -4 -8 11318.4 843.103 2 2 -4 -8 29561.4 2000.42 1 2 -4 -8 30545.8 1243.00 2 1 -4 -8 3039.20 647.937 1 0 -4 -8 2226.51 553.349 1 -1 -4 -8 566.015 324.356 1 -2 -4 -8 12461.6 1334.44 1 -3 -4 -8 1091.08 405.475 1 -4 -4 -8 12469.1 1373.12 1 -5 -4 -8 4100.58 825.667 1 -6 -4 -8 3742.76 783.646 1 -7 -4 -8 228.623 266.953 1 11 -5 -8 1607.55 549.634 2 10 -5 -8 1537.45 468.692 2 9 -5 -8 860.520 368.416 2 9 -5 -8 1353.81 571.213 1 8 -5 -8 307.831 237.829 2 8 -5 -8 24.4870 149.198 1 7 -5 -8 2270.76 519.691 2 7 -5 -8 1398.32 530.802 1 6 -5 -8 5244.28 749.616 2 6 -5 -8 4310.44 853.669 1 5 -5 -8 172.095 230.787 1 5 -5 -8-66.7514 153.285 2 4 -5 -8 3185.16 774.639 1 4 -5 -8 3540.67 551.021 2 3 -5 -8 1571.13 526.586 1 3 -5 -8 914.809 246.953 2 2 -5 -8 4921.71 861.002 1 1 -5 -8 1164.13 401.598 1 0 -5 -8 58.2230 299.982 1 -1 -5 -8 9536.17 1209.38 1 -2 -5 -8 3787.67 783.192 1 -3 -5 -8 1393.49 464.791 1 -4 -5 -8 5931.89 1012.03 1 -5 -5 -8 2017.68 599.407 1 10 -6 -8 150.271 214.997 2 9 -6 -8-290.506 287.858 2 8 -6 -8 9651.44 1178.21 2 7 -6 -8 500.367 296.219 2 7 -6 -8 154.282 196.502 1 6 -6 -8 2960.08 585.442 2 6 -6 -8 2660.14 661.530 1 5 -6 -8 13582.9 1181.16 2 5 -6 -8 15147.5 1607.93 1 4 -6 -8 7204.61 1104.65 1 3 -6 -8 280.846 232.146 1 2 -6 -8 536.657 600.368 1 1 -6 -8 15037.6 1581.79 1 0 -6 -8-52.0173 154.181 1 -1 -6 -8 980.814 428.561 1 -2 -6 -8 89.6107 202.892 1 -3 -6 -8 7191.25 1113.51 1 9 -7 -8 429.985 342.007 2 8 -7 -8 181.742 201.466 2 7 -7 -8 2509.96 624.258 2 3 -7 -8 13268.5 1551.76 1 2 -7 -8 3889.90 807.037 1 1 -7 -8 538.503 271.831 1 12 0 -9 243.640 265.458 2 11 0 -9 303.639 278.711 2 10 0 -9-243.367 241.263 2 9 0 -9-135.370 271.453 2 8 0 -9-54.5904 215.692 2 7 0 -9-45.8379 216.856 2 7 0 -9-80.7941 264.715 1 6 0 -9 239.757 250.551 2 6 0 -9 4.74326 158.430 1 5 0 -9 365.780 309.619 1 4 0 -9 300.266 202.458 1 3 0 -9-27.6142 162.765 1 2 0 -9 63.4391 175.032 1 1 0 -9-165.637 176.709 1 0 0 -9 88.0558 178.714 1 -1 0 -9-25.6497 167.213 1 -2 0 -9-854.677 317.843 1 -3 0 -9-71.7909 219.196 1 -4 0 -9-110.615 174.889 1 -5 0 -9 167.543 178.064 1 -6 0 -9 205.409 165.846 1 -7 0 -9 454.865 276.451 1 -8 0 -9-510.032 315.169 1 12 -1 -9 2534.79 699.705 2 11 1 -9 4961.25 956.347 2 11 -1 -9 4020.51 810.630 2 10 1 -9 1993.98 635.588 2 10 -1 -9 1580.05 521.638 2 9 1 -9 5447.40 923.320 2 9 -1 -9 5068.26 866.499 2 8 -1 -9 2394.30 576.614 2 8 -1 -9 3200.41 699.680 1 7 -1 -9 2859.52 604.558 2 7 -1 -9 3882.12 721.156 1 6 -1 -9 15730.4 1300.99 2 6 -1 -9 18659.4 1529.76 1 5 -1 -9 2927.12 546.360 2 5 1 -9 3214.10 556.450 1 5 -1 -9 3512.85 654.832 1 4 -1 -9 462.984 222.661 1 4 -1 -9 579.888 244.023 2 4 1 -9 592.776 251.496 1 3 -1 -9 127.915 203.913 1 3 -1 -9 26.3338 138.141 2 -3 -1 9 120.946 151.920 1 3 1 -9-5.06697 97.6763 1 2 1 -9-352.860 200.562 1 -2 -1 9-351.556 189.975 1 2 -1 -9 57.6746 198.592 1 2 -1 -9-5.20684 84.2973 2 1 1 -9 5460.01 686.802 1 1 -1 -9 6339.54 617.063 2 1 -1 -9 6279.46 833.416 1 -1 -1 9 6100.09 697.229 1 0 -1 -9 5836.57 541.513 2 0 1 -9 5735.76 706.038 1 0 -1 -9 5751.29 803.012 1 0 -1 9 5578.52 683.810 1 -1 -1 -9 220.809 101.110 2 -1 1 -9 76.4102 107.401 1 -1 -1 -9 333.278 174.560 1 -2 1 -9 3097.97 540.882 1 -2 -1 -9 3161.63 614.073 1 -3 1 -9 3920.69 614.123 1 -3 -1 -9 3629.12 671.596 1 -4 1 -9-79.8052 167.591 1 -4 -1 -9 19.8650 130.987 1 -5 1 -9 658.566 336.000 1 -5 -1 -9 73.9405 216.347 1 -6 1 -9 1085.01 368.126 1 -6 -1 -9 749.535 370.967 1 -7 1 -9 621.512 373.014 1 -7 -1 -9 711.075 354.596 1 -8 -1 -9 167.622 232.913 1 12 -2 -9 3281.58 722.503 2 11 2 -9 992.795 414.719 2 11 -2 -9 273.394 241.864 2 10 -2 -9-692.495 338.784 2 9 -2 -9-441.217 274.978 2 8 -2 -9 9089.38 1079.72 2 8 -2 -9 9198.13 1210.10 1 7 -2 -9 13161.8 1237.21 2 7 -2 -9 14077.0 1439.91 1 6 -2 -9 604.923 254.424 2 6 -2 -9 773.955 360.543 1 5 -2 -9 9313.42 949.894 2 5 -2 -9 10103.1 1164.37 1 4 -2 -9 1707.91 451.070 1 -4 -2 9 1923.90 376.264 1 4 -2 -9 2048.22 421.934 2 4 2 -9 2708.07 473.639 1 3 -2 -9 3755.55 521.630 2 3 -2 -9 3282.15 646.810 1 -3 -2 9 3279.05 472.538 1 3 2 -9 3450.25 506.856 1 2 -2 -9 3400.31 460.330 2 2 -2 -9 3842.07 704.465 1 -2 -2 9 3011.68 443.113 1 2 2 -9 3483.90 504.450 1 1 2 -9 601.465 201.295 1 1 -2 -9 482.561 281.351 1 1 -2 -9 406.673 147.642 2 0 2 -9 1619.51 336.127 1 0 -2 -9 974.756 331.623 1 -1 2 -9 8724.62 795.824 1 -1 -2 -9 8112.04 1023.35 1 -2 2 -9 6374.10 687.812 1 -2 -2 -9 5128.10 826.594 1 -3 2 -9 736.418 283.497 1 -3 -2 -9 13.2935 133.643 1 -4 2 -9 398.302 203.575 1 -4 -2 -9 325.431 193.482 1 -5 -2 -9 401.353 386.415 1 -6 -2 -9 151.704 193.320 1 -7 -2 -9-536.689 331.091 1 11 -3 -9 176.487 207.062 2 10 -3 -9 930.740 399.819 2 9 -3 -9 2221.53 573.947 2 9 -3 -9 1966.11 593.772 1 8 -3 -9 278.655 274.557 2 8 -3 -9 352.817 215.901 1 7 -3 -9-199.961 153.747 2 7 -3 -9 70.7231 197.240 1 6 -3 -9 44.1828 160.394 2 6 -3 -9-31.9673 195.025 1 5 -3 -9 177.837 284.337 1 5 -3 -9 125.197 141.689 2 4 -3 -9 445.381 316.438 1 4 -3 -9 82.3159 89.2624 2 3 -3 -9 902.969 384.500 1 3 -3 -9 743.253 250.646 2 2 -3 -9 235.025 208.519 1 2 -3 -9 34.6376 74.5269 2 1 -3 -9 2592.24 637.121 1 0 -3 -9 238.211 170.224 1 -1 -3 -9 29.0292 139.607 1 -2 -3 -9 326.280 190.542 1 -3 -3 -9 129.134 172.899 1 -4 -3 -9 3257.11 717.335 1 -5 -3 -9 430.719 310.142 1 -6 -3 -9 493.372 310.332 1 11 -4 -9 235.479 153.523 2 10 -4 -9-131.183 205.611 2 9 -4 -9 14592.0 1455.72 2 9 -4 -9 17795.7 1806.51 1 8 -4 -9 6167.47 897.494 2 8 -4 -9 9563.28 1320.56 1 7 -4 -9-37.3032 135.582 2 7 -4 -9 303.342 325.394 1 6 -4 -9 715.803 348.696 2 6 -4 -9 499.382 313.120 1 5 -4 -9 850.407 435.415 1 5 -4 -9 850.013 283.081 2 4 -4 -9 4610.63 882.458 1 4 -4 -9 2973.56 489.398 2 3 -4 -9 4177.00 818.923 1 2 -4 -9 2013.53 542.760 1 1 -4 -9 783.201 284.163 1 0 -4 -9 2879.20 666.313 1 -1 -4 -9 193.258 188.595 1 -2 -4 -9-200.982 287.252 1 -3 -4 -9 164.589 181.052 1 -4 -4 -9-4.16596 261.745 1 -5 -4 -9 2020.63 599.956 1 10 -5 -9 3578.84 783.461 2 9 -5 -9 1194.61 422.536 2 8 -5 -9 237.188 149.526 2 7 -5 -9 7317.52 938.419 2 7 -5 -9 11960.3 1475.99 1 6 -5 -9 9788.24 1025.18 2 6 -5 -9 8773.45 1269.97 1 5 -5 -9 2843.64 686.200 1 4 -5 -9 3589.69 789.634 1 3 -5 -9-65.2704 209.033 1 2 -5 -9 5856.32 1006.76 1 1 -5 -9 2946.41 722.862 1 0 -5 -9 5369.93 965.487 1 -1 -5 -9 637.334 416.023 1 -2 -5 -9 398.185 313.087 1 -3 -5 -9-669.715 392.042 1 9 -6 -9 1502.02 491.310 2 8 -6 -9 3795.67 750.818 2 4 -6 -9 249.857 415.900 1 3 -6 -9-61.0603 206.840 1 2 -6 -9 3602.65 825.515 1 1 -6 -9 1064.14 517.391 1 11 0 -10 607.075 345.040 2 10 0 -10-740.083 371.403 2 9 0 -10 4791.07 848.554 2 8 0 -10 426.297 264.219 2 7 0 -10 9787.71 1153.33 2 7 0 -10 12620.5 1318.17 1 6 0 -10 129.012 179.523 2 6 0 -10 175.690 226.106 1 5 0 -10 23899.9 1695.66 1 4 0 -10-80.9889 217.064 1 3 0 -10 10233.8 1090.94 1 2 0 -10 19013.1 1498.27 1 1 0 -10 16734.0 1345.88 1 0 0 -10 33.3384 210.106 1 -1 0 -10 3052.35 607.484 1 -2 0 -10 20078.0 1543.21 1 -3 0 -10-43.1805 233.572 1 -4 0 -10 482.079 309.071 1 -5 0 -10-285.142 225.689 1 -6 0 -10 2794.87 642.112 1 11 -1 -10 5444.24 986.055 2 10 1 -10 1088.53 450.670 2 10 -1 -10 1623.09 511.569 2 9 1 -10 126.012 171.762 2 9 -1 -10 309.035 321.088 2 8 -1 -10-398.376 256.503 2 8 -1 -10 289.245 206.828 1 7 -1 -10 18174.6 1548.71 2 7 -1 -10 15939.3 1517.56 1 6 -1 -10 1213.42 363.938 2 6 -1 -10 1028.80 417.334 1 5 -1 -10 10914.0 1081.46 2 5 1 -10 11744.2 1133.59 1 4 -1 -10 5034.53 817.482 1 4 -1 -10 6866.68 807.970 2 4 1 -10 7790.56 898.722 1 3 -1 -10 11649.7 994.015 2 3 1 -10 9702.97 985.057 1 2 1 -10 208.390 186.743 1 2 -1 -10 62.0875 148.228 1 2 -1 -10 519.838 179.275 2 1 1 -10 2373.18 506.955 1 1 -1 -10 1216.83 404.974 1 0 1 -10 11125.0 1037.21 1 0 -1 -10 7639.65 992.106 1 -1 1 -10 1601.94 415.619 1 -1 -1 -10 650.503 271.903 1 -2 1 -10 3601.08 610.983 1 -2 -1 -10 3406.26 671.358 1 -3 1 -10 246.741 213.711 1 -3 -1 -10 127.782 232.978 1 -4 -1 -10 4574.77 800.209 1 -5 -1 -10 907.819 322.507 1 -6 -1 -10 1063.67 426.843 1 -7 -1 -10 1991.25 550.647 1 11 -2 -10 7.11570 164.673 2 10 -2 -10 3249.05 727.679 2 9 -2 -10 378.322 315.023 2 9 -2 -10 738.779 345.160 1 8 -2 -10 6999.99 972.073 2 8 -2 -10 7740.28 1125.79 1 7 -2 -10 2539.31 561.804 2 7 -2 -10 3267.03 715.230 1 6 -2 -10 174.280 174.495 2 6 -2 -10-699.682 354.510 1 5 -2 -10 20550.0 1434.05 2 5 -2 -10 14542.6 1469.23 1 4 -2 -10 8816.10 886.801 2 4 2 -10 8521.63 877.607 1 3 -2 -10 3375.23 721.445 1 3 -2 -10 4763.37 606.357 2 3 2 -10 4671.88 627.494 1 2 -2 -10 4182.67 786.156 1 2 2 -10 6470.35 719.809 1 1 -2 -10 751.104 343.952 1 1 2 -10 675.891 248.086 1 0 -2 -10 4163.23 766.489 1 -1 -2 -10 576.481 294.266 1 -2 -2 -10 2416.11 589.179 1 -3 -2 -10 3323.65 751.269 1 -4 -2 -10 657.649 379.151 1 -5 -2 -10 8763.52 1179.97 1 -6 -2 -10-296.106 276.289 1 11 -3 -10 1333.15 541.337 2 10 -3 -10 9898.57 1253.18 2 9 -3 -10 426.275 269.919 2 9 -3 -10 69.9453 232.792 1 8 -3 -10 651.898 281.353 2 8 -3 -10 167.804 231.746 1 7 -3 -10 3308.47 671.037 2 7 -3 -10 2807.77 693.400 1 6 -3 -10 12725.7 1189.26 2 6 -3 -10 12971.9 1462.76 1 5 -3 -10 1636.80 415.860 1 5 -3 -10 1488.61 379.261 2 4 -3 -10 1336.38 472.787 1 3 -3 -10 1027.55 416.296 1 2 -3 -10 18465.9 1683.97 1 1 -3 -10 3178.65 688.427 1 0 -3 -10 1265.13 470.047 1 -1 -3 -10 3945.53 780.292 1 -2 -3 -10 4583.58 856.912 1 -3 -3 -10 6303.92 1043.27 1 -4 -3 -10 388.933 302.080 1 10 -4 -10 3926.11 796.302 2 9 -4 -10-413.624 277.526 2 8 -4 -10 10076.6 1178.76 2 7 -4 -10 2548.61 563.060 2 7 -4 -10 2130.31 604.457 1 6 -4 -10 356.106 353.676 1 5 -4 -10 588.480 354.428 1 4 -4 -10 8831.85 1248.01 1 3 -4 -10 2189.75 625.986 1 2 -4 -10 602.066 347.683 1 1 -4 -10 1411.26 499.544 1 0 -4 -10 2585.83 667.684 1 -1 -4 -10 151.436 223.194 1 -2 -4 -10 787.285 405.507 1 3 -5 -10 7172.86 1167.50 1 2 -5 -10 2609.87 679.918 1 10 0 -11 951.529 407.426 2 9 0 -11-548.541 330.577 2 8 0 -11-859.711 387.811 2 7 0 -11-39.8921 279.972 2 7 0 -11-119.946 314.156 1 6 0 -11-82.7204 241.002 2 6 0 -11 38.2840 218.389 1 5 0 -11-310.988 219.737 2 5 0 -11 76.1044 264.966 1 4 0 -11-257.343 192.278 2 4 0 -11 3.23366 252.193 1 3 0 -11-38.2046 149.262 1 2 0 -11-691.265 319.657 1 1 0 -11 162.086 148.899 1 0 0 -11-1.03956 129.183 1 -1 0 -11 575.684 323.766 1 -2 0 -11-59.6917 162.045 1 10 -1 -11-395.201 281.090 2 9 1 -11 508.150 352.883 2 9 -1 -11 574.552 332.053 2 8 1 -11 450.206 359.895 2 8 -1 -11 730.357 338.297 2 8 -1 -11 503.621 332.236 1 7 -1 -11 2445.12 602.442 2 7 -1 -11 2288.95 641.523 1 6 -1 -11 1476.97 438.225 2 6 -1 -11 1463.83 482.716 1 5 -1 -11 486.250 242.632 2 5 1 -11 262.242 213.500 1 5 -1 -11 45.3731 161.331 1 4 -1 -11 1081.52 402.712 2 4 1 -11 1178.59 432.387 1 4 -1 -11 1110.22 450.197 1 3 -1 -11-219.634 208.648 1 3 1 -11-129.450 174.791 1 2 -1 -11 1150.34 480.891 1 2 1 -11 240.489 198.218 1 1 -1 -11 1357.53 456.857 1 0 -1 -11 345.433 244.894 1 -1 -1 -11 764.620 373.492 1 -2 -1 -11 986.335 419.831 1 -3 -1 -11 113.160 380.311 1 -4 -1 -11-430.328 306.070 1 10 -2 -11 1580.48 517.791 2 9 -2 -11 2634.59 611.697 2 8 -2 -11 2992.38 643.852 2 8 -2 -11 2334.55 670.558 1 7 -2 -11-339.791 239.562 2 7 -2 -11-121.860 264.090 1 6 -2 -11 1486.94 402.216 2 6 -2 -11-148.832 210.035 1 5 -2 -11 376.486 393.116 1 4 -2 -11 401.584 301.622 1 3 -2 -11-335.373 271.196 1 2 -2 -11 133.481 169.293 1 1 -2 -11 179.810 217.173 1 0 -2 -11 4266.63 851.118 1 -1 -2 -11 69.5267 177.525 1 -2 -2 -11-248.154 260.812 1 -3 -2 -11 537.959 355.117 1 -4 -2 -11-787.147 428.396 1 10 -3 -11 1517.79 488.619 2 9 -3 -11-116.581 270.163 2 8 -3 -11 28.0376 154.141 2 6 -3 -11 186.064 250.963 1 5 -3 -11-263.301 252.964 1 4 -3 -11-785.771 401.334 1 3 -3 -11 675.024 365.119 1 2 -3 -11 720.066 365.243 1 1 -3 -11 562.106 338.494 1 0 -3 -11 92.3760 226.225 1 -1 -3 -11-560.946 362.022 1 -2 -3 -11-1990.48 607.122 1 8 0 -12 4745.86 885.783 2 7 0 -12 1314.60 461.491 2 6 0 -12 17660.4 1599.19 2 6 0 -12 20285.4 1753.59 1 5 0 -12-250.406 252.140 1 4 0 -12 3310.80 710.602 1 8 1 -12 1094.75 451.867 2 8 -1 -12 950.378 403.369 2 7 1 -12 2331.38 606.564 2 7 -1 -12 2693.08 716.718 1 6 -1 -12 3794.31 800.864 1 5 -1 -12 3617.11 751.700 1 4 -1 -12 12512.7 1402.14 1 3 -1 -12 269.030 220.871 1 2 -1 -12 2865.04 696.263 1 1 -1 -12 732.743 368.313 1 0 -1 -12 3372.83 697.436 1 -1 -1 -12 486.981 314.885 1 5 -2 -12 3505.34 743.128 1 4 -2 -12-4.39891 258.103 1 3 -2 -12-1138.83 469.872 1 2 -2 -12 149.052 236.454 1 1 -2 -12 6355.57 1056.99 1 0 -2 -12 1310.16 500.602 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 43595 _shelx_shelxl_version_number 2016/6 _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 S1 S 0.89461(8) 0.09931(12) 0.66050(11) 0.0358(3) Uani 1 1 d . . . . . S2 S 0.63769(12) 0.75801(15) 0.51478(11) 0.0549(4) Uani 1 1 d . . . . . O2 O 1.0395(2) 0.2787(3) 0.5449(3) 0.0382(6) Uani 1 1 d . . . . . O1 O 0.7001(2) 0.1555(4) 0.7373(3) 0.0447(7) Uani 1 1 d . . . . . N1 N 0.8780(2) 0.4132(4) 0.5691(3) 0.0319(7) Uani 1 1 d . . . . . H1 H 0.895520 0.512229 0.533265 0.038 Uiso 1 1 calc R . . . . C3 C 0.7711(3) 0.3940(5) 0.6151(4) 0.0318(8) Uani 1 1 d . . . . . H3 H 0.708487 0.402838 0.526593 0.038 Uiso 1 1 calc R . . . . C2 C 0.9489(3) 0.2822(4) 0.5810(4) 0.0284(8) Uani 1 1 d . . . . . C1 C 0.7720(3) 0.2140(5) 0.6799(4) 0.0329(8) Uani 1 1 d . . . . . C4 C 0.7538(3) 0.5263(5) 0.7277(4) 0.0348(8) Uani 1 1 d . . . . . H4A H 0.815833 0.516961 0.815182 0.042 Uiso 1 1 calc R . . . . H4B H 0.682599 0.500960 0.759895 0.042 Uiso 1 1 calc R . . . . C5 C 0.7496(3) 0.7106(5) 0.6685(5) 0.0411(9) Uani 1 1 d . . . . . H5A H 0.821906 0.735326 0.638935 0.049 Uiso 1 1 calc R . . . . H5B H 0.743379 0.790242 0.750028 0.049 Uiso 1 1 calc R . . . . C6 C 0.5210(4) 0.7809(7) 0.6064(6) 0.0636(14) Uani 1 1 d . . . . . H6A H 0.454042 0.816835 0.534679 0.095 Uiso 1 1 calc GR . . . . H6B H 0.539135 0.867947 0.684339 0.095 Uiso 1 1 calc GR . . . . H6C H 0.506370 0.670273 0.650042 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 S1 0.0379(5) 0.0251(5) 0.0488(6) 0.0092(4) 0.0188(4) 0.0022(4) S2 0.0837(9) 0.0479(7) 0.0367(6) 0.0045(5) 0.0205(5) 0.0055(6) O2 0.0315(14) 0.0325(14) 0.0569(16) 0.0115(12) 0.0239(12) 0.0067(11) O1 0.0402(15) 0.0384(15) 0.0632(18) 0.0096(14) 0.0288(14) -0.0057(13) N1 0.0281(15) 0.0238(15) 0.0489(18) 0.0098(13) 0.0198(13) 0.0018(12) C3 0.0300(18) 0.0316(19) 0.0372(19) 0.0045(16) 0.0145(15) -0.0002(15) C2 0.0313(18) 0.0264(18) 0.0280(17) 0.0029(14) 0.0077(14) 0.0004(15) C1 0.0333(19) 0.0298(19) 0.0371(19) 0.0000(16) 0.0107(16) -0.0038(16) C4 0.035(2) 0.036(2) 0.0346(19) -0.0012(16) 0.0117(15) -0.0031(17) C5 0.041(2) 0.029(2) 0.061(2) -0.0012(18) 0.0293(19) -0.0010(17) C6 0.037(2) 0.083(4) 0.066(3) 0.021(3) 0.001(2) -0.005(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 S1 C2 91.75(16) . . ? C5 S2 C6 100.9(2) . . ? C3 N1 H1 119.9 . . ? C2 N1 H1 119.9 . . ? C2 N1 C3 120.1(3) . . ? N1 C3 H3 109.2 . . ? N1 C3 C1 106.0(3) . . ? N1 C3 C4 113.0(3) . . ? C1 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C4 C3 C1 110.1(3) . . ? O2 C2 S1 121.8(3) . . ? O2 C2 N1 127.3(3) . . ? N1 C2 S1 110.9(2) . . ? O1 C1 S1 123.8(3) . . ? O1 C1 C3 125.2(3) . . ? C3 C1 S1 111.1(2) . . ? C3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 . . ? C3 C4 C5 112.9(3) . . ? H4A C4 H4B 107.8 . . ? C5 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? S2 C5 H5A 108.3 . . ? S2 C5 H5B 108.3 . . ? C4 C5 S2 116.1(3) . . ? C4 C5 H5A 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? S2 C6 H6A 109.5 . . ? S2 C6 H6B 109.5 . . ? S2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C2 1.785(3) . ? S1 C1 1.775(4) . ? S2 C5 1.794(5) . ? S2 C6 1.802(5) . ? O2 C2 1.214(4) . ? O1 C1 1.199(4) . ? N1 H1 0.8800 . ? N1 C3 1.453(4) . ? N1 C2 1.323(4) . ? C3 H3 1.0000 . ? C3 C1 1.519(5) . ? C3 C4 1.508(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.529(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ?