#------------------------------------------------------------------------------ #$Date: 2020-03-04 03:42:46 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248713 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557311.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_1557311 loop_ _publ_author_name 'Steinbiss, Michael' 'Maczka, Michael' 'Langewald, Juergen' 'London, Brecht' 'Vallinayagam, Ramakrishnan' 'Jones, Peter G.' 'Bastiaans, Harold' 'Schulz, Stefan' _publ_section_title ; Sigillins from Springtails Are Potent Natural Insecticides. ; _journal_issue 2 _journal_name_full 'Journal of natural products' _journal_page_first 468 _journal_page_last 472 _journal_paper_doi 10.1021/acs.jnatprod.9b01013 _journal_volume 83 _journal_year 2020 _chemical_formula_sum 'C12 H13 Cl5 O2' _chemical_formula_weight 366.47 _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 90 _cell_angle_beta 99.613(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.0710(4) _cell_length_b 9.5329(2) _cell_length_c 17.7642(5) _cell_measurement_reflns_used 27892 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.4720 _cell_measurement_theta_min 2.3890 _cell_volume 3017.25(13) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-2017 _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.1419 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur, Eos' _diffrn_measurement_method \w-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_unetI/netI 0.0223 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 132448 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 30.000 _diffrn_reflns_theta_max 30.031 _diffrn_reflns_theta_min 2.286 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.207 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 345 _refine_ls_number_reflns 8782 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0348 _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^)+(0.0244P)^2^+2.8034P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.0763 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7641 _reflns_number_total 8782 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file np9b01013_si_002.cif _cod_data_source_block slaus _cod_depositor_comments 'Adding full bibliography for 1557311--1557312.cif.' _cod_original_cell_volume 3017.26(13) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557311 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.731 _shelx_estimated_absorpt_t_max 0.796 _shelx_res_file ; TITL slaus in P2(1)/c shelx.res created by SHELXL-2017/1 at 12:54:24 on 31-Jul-2019 CELL 0.71073 18.070958 9.532934 17.764238 90.0000 99.6133 90.0000 ZERR 8.00 0.0004 0.0002 0.0005 0.0000 0.003 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H O Cl UNIT 96 104 16 40 TEMP -173 SIZE 0.35 0.35 0.25 FMAP 2 PLAN 10 L.S. 4 SHEL 999 0.71 ACTA 60 CONF WGHT 0.024400 2.803400 FVAR 1.80282 C1 1 0.643969 0.062004 0.594986 11.00000 0.00880 0.01417 = 0.02703 -0.00363 0.00133 0.00028 AFIX 13 H1 2 0.649868 0.069074 0.540136 11.00000 -1.20000 AFIX 0 C2 1 0.653149 0.209497 0.630317 11.00000 0.01213 0.02035 = 0.05754 -0.01601 0.00028 -0.00019 AFIX 23 H2A 2 0.694676 0.207997 0.674391 11.00000 -1.20000 H2B 2 0.667099 0.275702 0.592093 11.00000 -1.20000 AFIX 0 C3 1 0.582361 0.262231 0.656842 11.00000 0.01443 0.01836 = 0.02340 -0.00889 -0.00500 0.00384 AFIX 13 H3 2 0.578073 0.211695 0.705255 11.00000 -1.20000 AFIX 0 C4 1 0.586846 0.418990 0.675124 11.00000 0.01659 0.02039 = 0.04626 -0.01931 -0.00961 0.00407 AFIX 23 H4A 2 0.594784 0.471530 0.629065 11.00000 -1.20000 H4B 2 0.630501 0.436700 0.715681 11.00000 -1.20000 AFIX 0 C5 1 0.515461 0.472920 0.701554 11.00000 0.02769 0.02469 = 0.02649 -0.01434 -0.00903 0.01144 AFIX 23 H5A 2 0.512516 0.434049 0.752649 11.00000 -1.20000 H5B 2 0.517737 0.576418 0.705916 11.00000 -1.20000 AFIX 0 C6 1 0.446738 0.431630 0.646750 11.00000 0.01834 0.01522 = 0.01318 -0.00198 0.00469 0.00339 C7 1 0.441529 0.277194 0.628557 11.00000 0.01597 0.01300 = 0.02102 0.00237 0.00647 0.00342 AFIX 23 H7A 2 0.396671 0.259281 0.589485 11.00000 -1.20000 H7B 2 0.435841 0.223940 0.675094 11.00000 -1.20000 AFIX 0 C8 1 0.512212 0.226312 0.598731 11.00000 0.01062 0.01066 = 0.01146 -0.00109 0.00099 0.00023 C9 1 0.507795 0.068030 0.591979 11.00000 0.01159 0.01212 = 0.01227 0.00016 0.00262 0.00209 C10 1 0.702275 -0.042566 0.634627 11.00000 0.01192 0.02247 = 0.01925 -0.00329 0.00192 0.00231 C11 1 0.393595 0.522230 0.617863 11.00000 0.01639 0.01250 = 0.01465 -0.00122 0.00480 0.00134 C12 1 0.513432 0.286479 0.519050 11.00000 0.02989 0.01334 = 0.01534 0.00143 0.00714 0.00103 AFIX 137 H12A 2 0.467483 0.259014 0.484745 11.00000 -1.50000 H12B 2 0.557168 0.249913 0.499385 11.00000 -1.50000 H12C 2 0.516428 0.389026 0.522010 11.00000 -1.50000 AFIX 0 O1 3 0.572991 -0.004528 0.598683 11.00000 0.00856 0.01270 = 0.02870 -0.00391 0.00143 0.00053 O2 3 0.450632 0.001206 0.583044 11.00000 0.01229 0.01267 = 0.03467 -0.00082 0.00571 -0.00108 CL1 4 0.691486 -0.207998 0.588511 11.00000 0.01760 0.01685 = 0.04396 -0.00572 0.00200 0.00501 CL2 4 0.693087 -0.065413 0.731584 11.00000 0.02258 0.06812 = 0.01896 0.00217 0.00166 0.00380 CL3 4 0.793254 0.021035 0.628490 11.00000 0.00953 0.02580 = 0.03454 -0.00551 0.00325 0.00135 CL4 4 0.395127 0.699149 0.638128 11.00000 0.02697 0.01238 = 0.01904 -0.00166 0.00645 0.00454 CL5 4 0.313387 0.475438 0.555223 11.00000 0.01867 0.02098 = 0.04170 -0.00656 -0.00722 0.00650 C1' 1 0.144372 0.058780 0.577613 11.00000 0.00905 0.01385 = 0.02003 -0.00130 0.00283 0.00095 AFIX 13 H1' 2 0.148829 0.041069 0.523065 11.00000 -1.20000 AFIX 0 C2' 1 0.154247 0.217427 0.591970 11.00000 0.01263 0.01278 = 0.02901 -0.00138 0.00754 -0.00097 AFIX 23 H2'1 2 0.205491 0.235240 0.619984 11.00000 -1.20000 H2'2 2 0.149318 0.266383 0.542233 11.00000 -1.20000 AFIX 0 C3' 1 0.097428 0.278478 0.637418 11.00000 0.01090 0.01234 = 0.01609 -0.00213 0.00025 0.00022 AFIX 13 H3' 2 0.108576 0.239058 0.690266 11.00000 -1.20000 AFIX 0 C4' 1 0.103747 0.438341 0.643588 11.00000 0.01264 0.01243 = 0.02732 -0.00408 0.00039 -0.00218 AFIX 23 H4'1 2 0.096962 0.479182 0.591650 11.00000 -1.20000 H4'2 2 0.154633 0.463625 0.670036 11.00000 -1.20000 AFIX 0 C5' 1 0.045038 0.501568 0.687403 11.00000 0.01826 0.01602 = 0.02156 -0.00594 0.00078 0.00092 AFIX 23 H5'1 2 0.057839 0.476488 0.742112 11.00000 -1.20000 H5'2 2 0.045745 0.605103 0.683240 11.00000 -1.20000 AFIX 0 C6' 1 -0.032419 0.447747 0.655745 11.00000 0.01617 0.01249 = 0.01447 -0.00087 0.00563 0.00086 C7' 1 -0.038242 0.290468 0.650774 11.00000 0.01477 0.01125 = 0.02198 0.00200 0.00661 0.00207 AFIX 23 H7'1 2 -0.089920 0.263370 0.627580 11.00000 -1.20000 H7'2 2 -0.027370 0.249613 0.702684 11.00000 -1.20000 AFIX 0 C8' 1 0.017808 0.232796 0.602054 11.00000 0.01012 0.00857 = 0.01397 0.00024 0.00104 -0.00019 C9' 1 0.013167 0.074419 0.601725 11.00000 0.01155 0.01080 = 0.01704 -0.00002 0.00089 0.00162 C10' 1 0.204328 -0.031014 0.627456 11.00000 0.01163 0.01527 = 0.02459 0.00058 0.00380 0.00067 C11' 1 -0.090988 0.531017 0.633532 11.00000 0.01818 0.01306 = 0.01583 -0.00073 0.00478 0.00157 C12' 1 -0.005586 0.278631 0.518268 11.00000 0.02375 0.01391 = 0.01475 0.00028 -0.00169 -0.00007 AFIX 137 H12D 2 0.025799 0.230465 0.486392 11.00000 -1.50000 H12E 2 0.000925 0.380266 0.514275 11.00000 -1.50000 H12F 2 -0.058360 0.254309 0.500854 11.00000 -1.50000 AFIX 0 O1' 3 0.073932 -0.000087 0.590208 11.00000 0.00834 0.01135 = 0.03404 -0.00269 0.00306 -0.00035 O2' 3 -0.042057 0.009005 0.609022 11.00000 0.01389 0.01244 = 0.03997 0.00003 0.00878 -0.00211 CL1' 4 0.189963 -0.211837 0.606651 11.00000 0.01494 0.01350 = 0.07120 0.00024 -0.00072 0.00236 CL2' 4 0.202732 -0.004175 0.725764 11.00000 0.02263 0.05035 = 0.02146 0.00949 0.00465 0.00833 CL3' 4 0.293884 0.015049 0.607334 11.00000 0.00962 0.02010 = 0.03126 -0.00076 0.00595 0.00106 CL4' 4 -0.089231 0.711389 0.642529 11.00000 0.02666 0.01160 = 0.02000 -0.00114 0.00458 0.00500 CL5' 4 -0.178680 0.470366 0.591566 11.00000 0.01545 0.02128 = 0.03206 -0.00376 -0.00083 0.00378 HKLF 4 REM slaus in P2(1)/c REM R1 = 0.0348 for 7641 Fo > 4sig(Fo) and 0.0433 for all 8782 data REM 345 parameters refined using 0 restraints END WGHT 0.0244 2.8034 REM Highest difference peak 1.207, deepest hole -0.634, 1-sigma level 0.070 Q1 1 0.7001 0.0165 0.7324 11.00000 0.05 1.21 Q2 1 0.3195 0.4621 0.5957 11.00000 0.05 0.77 Q3 1 0.6933 -0.2079 0.6323 11.00000 0.05 0.58 Q4 1 0.1924 -0.1992 0.5610 11.00000 0.05 0.50 Q5 1 0.2069 -0.0927 0.7291 11.00000 0.05 0.50 Q6 1 0.5086 0.1517 0.5931 11.00000 0.05 0.46 Q7 1 0.5121 0.2543 0.5577 11.00000 0.05 0.42 Q8 1 0.0141 0.1461 0.5989 11.00000 0.05 0.41 Q9 1 0.6516 0.1344 0.6114 11.00000 0.05 0.41 Q10 1 -0.1816 0.4676 0.5488 11.00000 0.05 0.40 ; _shelx_res_checksum 10285 _shelx_hkl_file ; -2 0 0 203.849 36.3569 2 0 0 230.699 35.8576 2 0 0 174.576 36.0335 2 0 0 130.232 33.9644 2 0 0 235.264 38.1888 -2 0 0 170.009 35.6767 -2 0 0 182.385 35.5296 2 0 0 369.176 43.9030 3 0 0 1408.24 110.613 3 0 0 1650.01 113.658 -3 0 0 1316.72 101.185 3 0 0 1443.21 108.137 3 0 0 1525.57 114.518 -3 0 0 1477.53 109.197 3 0 0 1277.30 104.320 -3 0 0 1371.95 105.299 3 0 0 1571.75 116.766 3 0 0 1342.77 109.402 -3 0 0 1518.40 113.872 -3 0 0 1445.45 113.722 -3 0 0 1345.24 109.304 3 0 0 1399.37 107.205 -3 0 0 1581.57 114.705 -3 0 0 1284.23 105.451 -3 0 0 1353.30 105.049 3 0 0 1607.82 117.329 3 0 0 1338.82 104.964 4 0 0 3580.07 200.364 -4 0 0 3572.49 205.482 -4 0 0 3542.65 193.038 -4 0 0 4033.46 208.312 -4 0 0 3735.93 210.233 -4 0 0 3722.60 208.245 -4 0 0 3439.41 198.022 -4 0 0 3773.40 141.768 -4 0 0 3452.59 204.370 4 0 0 4073.63 210.723 4 0 0 3299.71 193.805 4 0 0 3500.06 207.620 4 0 0 3409.39 200.045 4 0 0 3994.86 214.903 4 0 0 3386.71 205.013 4 0 0 3688.22 203.879 4 0 0 3659.21 208.787 -4 0 0 3216.68 200.313 5 0 0 189.847 61.4393 -5 0 0 291.255 68.7379 -5 0 0 265.284 72.4597 5 0 0 203.015 63.9968 -5 0 0 278.401 76.3436 -5 0 0 319.453 80.7251 -5 0 0 194.202 40.0744 -5 0 0 259.657 76.6619 -5 0 0 101.493 52.1722 -5 0 0 281.401 70.1817 5 0 0 96.4317 64.2980 5 0 0 347.293 83.1796 5 0 0 293.063 76.2861 -5 0 0 152.802 61.3998 5 0 0 328.467 79.5824 5 0 0 240.270 72.1012 5 0 0 203.220 71.9866 5 0 0 288.252 77.4865 6 0 0 45656.2 1257.64 6 0 0 48607.1 1294.98 -6 0 0 45744.3 1281.34 -6 0 0 47450.3 1103.48 6 0 0 50197.4 1309.23 -6 0 0 45938.9 1284.35 6 0 0 48604.3 1272.79 6 0 0 50502.9 1309.34 -6 0 0 43750.2 1237.71 -6 0 0 47626.9 1289.84 6 0 0 48872.1 1297.53 6 0 0 48445.5 1294.42 6 0 0 49162.9 1282.08 -6 0 0 47452.7 1287.73 -6 0 0 47160.2 1266.66 -6 0 0 49436.4 1277.46 6 0 0 47940.5 1268.06 -6 0 0 47156.0 1287.08 7 0 0 69.6357 70.4389 -7 0 0 150.488 107.883 -7 0 0 118.695 96.7081 -7 0 0 76.5799 82.4345 -7 0 0 155.638 96.4741 -7 0 0 183.721 76.2838 -7 0 0 55.7719 33.7148 7 0 0 245.345 106.691 7 0 0 166.472 91.7157 7 0 0 148.431 89.5113 7 0 0 252.131 111.798 8 0 0 298503. 6532.67 8 0 0 299734. 6535.91 -8 0 0 301589. 6499.16 -8 0 0 294109. 6562.57 8 0 0 281457. 6513.36 8 0 0 305489. 6578.43 -8 0 0 293817. 6562.15 -8 0 0 298410. 6570.00 -8 0 0 298151. 6269.36 8 0 0 312896. 6587.42 9 0 0 783.267 195.838 9 0 0 990.529 178.329 -9 0 0 531.192 150.775 -9 0 0 1072.79 219.326 9 0 0 499.917 149.494 -9 0 0 629.181 85.9120 -9 0 0 723.838 204.544 -9 0 0 758.793 207.596 -9 0 0 624.770 180.377 9 0 0 946.168 200.040 9 0 0 860.253 178.383 10 0 0 264521. 6065.71 10 0 0 271769. 6142.27 -10 0 0 270685. 6138.68 -10 0 0 275034. 6146.08 -10 0 0 252618. 6044.44 10 0 0 268607. 6098.07 -10 0 0 275730. 6152.22 10 0 0 277313. 6097.10 -10 0 0 279983. 6159.25 -10 0 0 274435. 5753.73 10 0 0 270125. 6141.39 11 0 0 1983.78 263.557 -11 0 0 1459.76 232.665 11 0 0 1233.16 224.815 11 0 0 1435.80 226.398 -11 0 0 1579.73 247.508 -11 0 0 1681.69 252.973 -11 0 0 1782.74 231.123 -11 0 0 1683.12 254.700 11 0 0 1769.31 254.030 -11 0 0 1323.32 125.590 11 0 0 1331.76 227.766 -12 0 0 11408.7 649.105 -12 0 0 11040.0 639.407 -12 0 0 10824.9 405.581 -12 0 0 11272.8 600.909 -12 0 0 12351.8 671.570 12 0 0 11259.6 642.382 12 0 0 10716.4 629.871 12 0 0 10968.0 618.295 12 0 0 10342.7 597.445 -12 0 0 10855.6 638.477 12 0 0 10633.1 608.624 -13 0 0 1751.60 274.980 13 0 0 1780.37 271.857 -13 0 0 1958.43 251.080 13 0 0 1757.67 253.256 13 0 0 1487.23 239.718 13 0 0 1761.94 274.730 -13 0 0 1477.59 249.774 13 0 0 1504.40 244.883 -13 0 0 1963.09 291.538 -13 0 0 1444.57 251.776 -13 0 0 1735.86 144.867 -14 0 0 483.919 183.258 -14 0 0 683.427 186.728 14 0 0 565.607 173.798 14 0 0 584.198 171.939 -14 0 0 510.034 81.6851 -14 0 0 882.393 197.354 14 0 0 718.387 192.403 -14 0 0 1032.81 228.973 14 0 0 571.767 146.264 -14 0 0 699.597 187.093 14 0 0 648.288 192.528 15 0 0 8702.85 602.494 -15 0 0 7929.97 606.237 15 0 0 8020.24 609.653 -15 0 0 8150.37 613.014 -15 0 0 7983.04 577.441 15 0 0 7811.72 586.531 15 0 0 7934.02 608.602 15 0 0 7696.77 574.066 -15 0 0 7684.46 596.113 -15 0 0 9033.31 644.691 -16 0 0 4223.25 458.464 16 0 0 4188.41 456.986 -16 0 0 4441.61 471.187 16 0 0 4043.26 425.229 -16 0 0 3579.68 409.804 -16 0 0 4244.31 457.558 16 0 0 4082.82 450.308 -16 0 0 4994.34 492.133 16 0 0 4394.60 447.798 16 0 0 4449.82 459.319 17 0 0 7767.09 616.758 17 0 0 8162.56 654.230 -17 0 0 8215.56 659.080 17 0 0 7138.05 600.283 17 0 0 7330.01 597.916 -17 0 0 8248.49 660.201 17 0 0 7018.85 610.796 -17 0 0 8077.33 655.566 -17 0 0 6827.05 559.657 -17 0 0 7416.94 627.800 -18 0 0 28850.4 1377.51 18 0 0 30772.2 1411.17 18 0 0 28257.1 1367.02 -18 0 0 32395.7 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154.749 4 10 0 246.754 149.262 4 -10 0 194.285 130.993 4 10 0 582.942 201.436 -4 -10 0 357.861 181.500 4 10 0 249.661 130.024 4 10 0 415.960 196.729 -5 10 0 197.107 120.156 -5 -10 0 230.202 137.002 -5 -10 0 142.222 158.960 5 10 0 463.352 204.494 -5 -10 0 566.878 186.339 5 10 0 200.040 115.350 -5 10 0 419.657 186.690 5 -10 0 409.519 197.254 -5 10 0 415.059 136.501 -5 10 0 183.780 149.562 5 10 0 448.169 186.372 5 -10 0 241.994 176.596 5 10 0 541.195 184.973 -5 10 0 342.353 133.744 -5 -10 0 617.656 206.114 5 10 0 80.5783 149.684 -5 10 0 325.447 128.612 5 -10 0 906.702 256.498 -6 -10 0 2001.66 331.666 -6 10 0 1964.41 276.879 6 -10 0 1942.60 364.899 6 10 0 2819.22 380.654 -6 10 0 2015.59 279.805 6 -10 0 1872.52 343.060 -6 -10 0 2549.15 349.908 6 -10 0 2371.79 381.842 -6 -10 0 1704.71 306.579 6 10 0 2005.36 359.372 6 10 0 2650.90 415.354 6 10 0 2390.65 348.977 6 10 0 2743.80 368.843 -6 10 0 2711.95 433.787 -6 10 0 2567.92 412.992 -6 10 0 2222.22 293.774 -6 -10 0 2306.85 382.189 -6 10 0 2050.75 283.357 7 10 0 1177.38 262.644 -7 10 0 1060.13 280.852 -7 -10 0 499.371 202.705 -7 -10 0 1019.55 282.031 -7 10 0 664.945 230.483 7 -10 0 815.692 252.749 7 10 0 1224.71 296.310 7 -10 0 1158.01 288.425 7 -10 0 728.563 251.449 7 10 0 587.008 204.826 -7 -10 0 755.807 217.078 7 10 0 909.701 266.553 7 10 0 859.179 218.831 -7 -10 0 940.779 256.290 8 10 0 7384.86 647.923 -8 10 0 8918.79 768.378 8 10 0 7804.15 713.069 -8 10 0 9162.56 787.108 -8 -10 0 8419.97 716.639 -8 -10 0 8785.06 667.079 8 10 0 6925.56 623.510 8 10 0 8028.02 716.895 8 -10 0 8129.34 698.501 8 -10 0 10088.0 800.111 -8 -10 0 7206.36 640.692 8 -10 0 8482.27 745.814 -8 -10 0 8242.24 689.746 -9 -10 0 834.168 249.498 9 -10 0 897.279 266.207 9 -10 0 419.112 209.296 9 10 0 1085.95 306.859 9 10 0 732.801 230.811 -9 -10 0 668.599 239.927 -9 10 0 433.090 207.755 -9 -10 0 768.772 206.758 -9 -10 0 770.716 253.264 9 -10 0 446.689 193.382 -9 10 0 193.107 159.287 9 10 0 422.688 213.196 -9 -10 0 505.190 202.706 9 10 0 507.602 203.136 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0-76.0874 120.730 0 -11 0 297.954 214.915 0 -11 0-29.1762 156.799 1 11 0 326.927 156.963 1 -11 0 115.060 160.111 1 -11 0 150.986 136.958 -1 11 0 709.259 228.663 -1 11 0 635.161 249.651 1 11 0 297.136 129.290 -1 -11 0 223.164 192.639 1 11 0 681.854 186.829 -1 -11 0 908.087 277.184 -1 -11 0 477.684 170.469 1 11 0 532.106 239.189 1 -11 0 1099.69 314.602 1 11 0 16.2359 112.538 -1 -11 0 280.114 158.808 2 -11 0 2425.08 407.930 -2 11 0 2703.27 425.578 2 11 0 2321.10 402.203 2 11 0 3163.08 383.514 2 -11 0 2391.36 409.207 -2 -11 0 2671.68 363.191 2 11 0 1907.79 336.045 2 11 0 3421.19 495.332 2 11 0 3050.13 381.165 2 -11 0 3213.90 445.037 -2 11 0 3397.31 483.958 2 11 0 3363.61 391.382 -2 -11 0 2237.48 386.024 -2 -11 0 2692.72 421.313 -3 11 0-61.4396 179.146 3 11 0 189.977 141.908 3 11 0-67.2712 146.467 3 11 0-10.9390 133.190 -3 11 0-33.5073 151.989 3 11 0 59.9856 108.292 3 -11 0 248.861 186.997 3 11 0-143.924 141.029 -3 -11 0-211.179 201.778 3 -11 0-15.9123 135.089 -3 -11 0 113.757 111.371 3 -11 0 80.9805 169.238 3 11 0-70.3269 99.6354 -3 -11 0 143.683 174.832 -4 -11 0 36340.2 1516.14 -4 -11 0 34259.8 1646.45 4 11 0 35226.5 1474.36 4 -11 0 35457.1 1653.38 -4 -11 0 31721.9 1529.68 4 11 0 36916.4 1494.95 4 11 0 36235.5 1481.17 4 11 0 36940.5 1697.59 4 11 0 34448.0 1652.18 4 11 0 35920.7 1575.95 4 -11 0 33388.1 1636.26 4 -11 0 34360.7 1597.38 -4 11 0 36541.2 1672.27 -4 11 0 36931.9 1717.12 5 -11 0 370.837 204.216 5 -11 0-8.87316 154.334 -5 11 0-22.0261 172.830 5 11 0 154.865 184.569 5 11 0 35.2244 107.077 5 11 0-59.7909 186.505 5 11 0-84.6548 131.741 -5 -11 0 2.96734 150.009 5 11 0 494.445 219.676 -5 -11 0 127.650 148.246 5 -11 0-205.732 204.507 -5 -11 0-143.367 166.269 -5 11 0 269.225 231.444 6 -11 0 28339.9 1494.64 6 11 0 28911.0 1372.81 -6 -11 0 27349.6 1267.74 6 -11 0 26528.6 1408.87 6 11 0 27092.9 1442.42 6 11 0 27834.9 1311.55 -6 11 0 29418.3 1535.24 -6 -11 0 28796.5 1385.82 6 -11 0 26048.1 1414.61 -6 -11 0 27543.1 1330.63 -6 -11 0 26939.4 1424.87 -6 11 0 28674.9 1485.51 6 11 0 28924.9 1487.72 6 11 0 28831.3 1332.78 7 11 0 962.721 293.003 7 -11 0 511.746 204.923 -7 -11 0 601.114 211.021 -7 11 0 514.017 251.102 7 11 0 452.050 172.165 -7 -11 0 704.373 255.657 7 11 0 643.119 201.848 -7 -11 0 358.648 180.200 7 11 0 771.007 228.488 7 -11 0 655.447 257.348 -7 11 0 623.168 229.036 7 11 0 248.142 201.596 -7 -11 0 747.259 223.922 7 -11 0 1080.98 284.773 -8 -11 0 263.163 201.274 -8 -11 0 529.057 211.140 -8 11 0 560.765 217.698 -8 -11 0 1141.94 270.613 8 11 0 751.029 263.005 -8 -11 0 497.018 194.150 8 11 0 778.839 271.402 8 -11 0 619.790 243.856 8 -11 0 354.167 181.835 8 11 0 662.279 225.089 -8 11 0 581.746 202.909 8 -11 0 406.627 193.319 -8 -11 0 527.704 196.260 8 11 0 663.526 233.843 9 -11 0 1122.59 287.078 -9 -11 0 2041.18 367.950 9 11 0 2023.69 353.271 -9 -11 0 1115.17 292.432 9 11 0 1338.28 323.749 -9 -11 0 1321.12 317.755 9 11 0 1637.07 361.509 -9 11 0 2436.29 433.770 -9 11 0 2406.41 443.651 -9 -11 0 2297.28 384.606 9 -11 0 1267.23 312.203 9 -11 0 1926.42 354.362 9 11 0 1127.27 276.225 -10 -11 0 505.925 217.001 -10 11 0 800.850 291.368 10 11 0 873.165 278.301 10 11 0 605.341 221.597 -10 -11 0 1102.23 293.787 10 -11 0 623.498 249.197 10 11 0 658.909 210.980 -10 11 0 1664.02 376.311 -10 -11 0 1199.92 303.754 10 -11 0 883.417 292.003 10 11 0 1088.28 335.561 -10 -11 0 1089.42 276.329 10 -11 0 1037.15 277.799 -11 -11 0 2135.54 385.861 -11 11 0 2442.89 451.820 -11 -11 0 2091.45 384.214 -11 11 0 2472.66 452.536 11 -11 0 1737.53 372.922 11 11 0 2889.29 437.116 11 -11 0 2401.26 441.477 -11 -11 0 1308.00 331.626 11 11 0 2497.43 449.163 11 11 0 2629.68 461.578 11 -11 0 1897.39 377.469 -11 -11 0 1594.68 333.741 11 11 0 2212.18 386.004 12 11 0 1830.60 371.621 12 11 0 3051.52 493.638 -12 -11 0 2419.42 421.685 12 -11 0 2672.44 466.446 -12 -11 0 2628.13 434.869 -12 -11 0 1799.70 350.507 -12 11 0 2459.11 456.772 -12 11 0 2733.01 474.569 12 -11 0 2941.77 483.121 -12 -11 0 3145.38 482.397 12 11 0 2349.54 415.187 12 -11 0 2488.99 414.353 12 11 0 2265.72 416.489 13 11 0 229.360 190.383 -13 -11 0 173.151 158.665 -13 -11 0 235.472 182.193 13 11 0 66.3626 139.082 -13 -11 0-160.393 204.710 13 11 0-136.644 182.708 13 11 0 33.9526 161.592 -13 -11 0-145.457 171.250 13 -11 0 688.313 264.690 -14 -11 0 12630.7 991.792 14 11 0 11341.4 943.455 -14 -11 0 12052.3 968.465 14 11 0 11192.9 938.140 -14 -11 0 10576.8 914.685 14 11 0 11211.7 949.609 15 11 0 1564.20 377.131 0 -12 0 10421.4 902.732 0 12 0 13564.2 1013.90 0 12 0 12244.4 930.001 0 -12 0 12377.3 962.502 0 -12 0 11663.3 886.116 -1 12 0 418.039 178.093 1 -12 0 898.233 276.276 1 -12 0 698.946 245.307 -1 12 0 729.293 257.608 1 -12 0 702.738 258.240 -1 -12 0 249.790 157.771 1 12 0 618.578 260.754 -1 -12 0 595.173 269.202 1 12 0 563.742 229.104 2 -12 0 2352.26 409.977 -2 -12 0 2632.79 453.652 2 -12 0 2067.67 415.007 -2 -12 0 2148.41 395.710 2 12 0 1945.95 371.332 -2 12 0 2135.10 390.580 2 12 0 1965.88 399.088 2 12 0 2201.53 415.199 2 -12 0 1689.69 394.908 -2 12 0 1987.60 397.597 -3 -12 0 25.1973 174.172 3 12 0 170.985 172.705 3 -12 0 85.3597 150.405 -3 -12 0 550.079 233.072 3 -12 0 551.418 264.626 3 -12 0 537.181 247.993 3 12 0 239.167 163.279 3 12 0 371.269 202.051 -3 12 0 403.093 245.464 -3 12 0 85.6678 164.209 -4 12 0 3003.12 486.372 4 12 0 2369.24 391.327 4 12 0 2833.82 476.992 -4 -12 0 2101.50 385.773 4 -12 0 2057.43 400.422 -4 -12 0 2702.62 467.426 4 12 0 2564.67 463.017 4 -12 0 2239.43 404.740 -4 12 0 2861.15 482.910 4 -12 0 2824.02 459.133 5 12 0 309.017 175.915 5 -12 0 12.4521 187.931 -5 -12 0 466.512 240.370 -5 12 0 203.533 213.609 5 12 0 37.1044 151.884 -5 12 0 373.169 123.104 5 -12 0 364.922 169.921 5 -12 0 249.771 168.572 5 12 0 490.421 237.446 -5 -12 0 259.782 132.383 -6 -12 0 1801.16 372.513 -6 12 0 984.768 303.790 6 -12 0 835.830 273.482 6 -12 0 688.305 261.599 -6 12 0 2004.53 410.355 -6 -12 0 1226.35 304.665 6 12 0 1731.31 345.247 6 12 0 2209.19 417.227 6 -12 0 964.196 307.312 6 12 0 1796.83 378.652 -7 12 0 963.941 306.619 7 12 0 921.081 281.211 7 -12 0 1395.02 355.308 7 -12 0 1114.94 294.822 -7 -12 0 877.587 302.611 7 12 0 1582.20 374.533 -7 -12 0 1307.49 303.586 7 -12 0 1757.02 368.443 7 12 0 886.607 237.195 -7 12 0 1075.46 342.440 8 -12 0 972.728 292.178 8 12 0 812.070 279.624 -8 -12 0 611.016 265.949 8 -12 0 759.271 267.708 8 12 0 1009.84 321.300 -8 12 0 657.848 260.472 -8 12 0 727.812 271.755 9 12 0 550.776 245.023 9 -12 0 1043.91 313.282 -9 12 0 1097.76 318.224 9 12 0 546.359 205.348 9 -12 0 733.859 253.299 -9 -12 0 621.828 251.498 -10 -12 0 8125.52 781.075 10 12 0 8127.85 808.183 10 -12 0 6821.24 723.956 11 12 0 1210.18 337.794 11 -12 0 1044.54 306.870 -11 -12 0 534.473 236.367 12 -12 0 621.762 251.280 -12 -12 0 273.999 197.625 -12 -12 0 609.681 252.474 0 -13 0 131.296 143.626 0 13 0 125.817 175.737 -1 13 0 406.548 237.013 1 -13 0 114.621 157.460 -1 -13 0 156.225 147.737 1 13 0-50.1853 142.996 -2 -13 0 4733.50 611.013 2 13 0 3815.58 539.010 2 -13 0 4533.84 591.653 -2 13 0 4979.96 626.091 3 13 0 822.591 272.689 -3 -13 0 1188.18 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1892.91 351.860 1 10 -10 1914.16 371.541 -1 10 10 1864.59 315.430 1 -10 -10 2550.64 435.783 -1 -10 10 2385.80 414.953 0 10 -10 403.991 194.859 0 10 -10 448.491 215.274 0 10 -10 553.885 231.999 0 -10 10 218.955 196.475 0 10 10 958.247 308.539 0 10 -10 565.417 207.595 0 -10 -10 344.647 181.711 0 10 -10 306.008 201.656 0 10 10 541.735 170.014 0 10 -10 813.018 270.565 0 -10 -10 386.477 243.452 0 -10 10 952.363 312.418 -1 10 -10 2418.67 412.775 -1 10 -10 2159.48 402.188 -1 10 -10 1794.92 363.886 1 -10 10 1952.92 396.921 1 10 10 2176.51 415.604 -1 10 -10 2640.84 424.729 -1 -10 -10 2086.41 361.604 -1 10 -10 2254.57 402.184 -1 10 -10 2282.14 407.459 -1 -10 -10 1760.41 356.481 1 -10 10 2244.45 425.408 -2 10 -10 663.987 226.174 -2 10 -10 724.394 256.721 -2 10 -10 267.544 207.829 2 10 10 485.835 218.551 -2 10 -10 222.336 161.606 -2 -10 -10 563.573 212.556 -2 10 -10 215.959 173.701 -2 10 -10 89.1965 168.757 2 -10 10 394.628 216.735 -2 -10 -10 383.358 212.622 2 -10 10 384.606 199.694 3 -10 10 2079.76 334.759 -3 10 -10 2029.53 386.435 -3 10 -10 1816.43 386.536 3 -10 10 1527.83 373.036 3 10 10 846.208 304.140 -3 10 -10 1729.94 351.219 -3 -10 -10 1600.69 323.908 -3 10 -10 826.161 250.608 -3 10 -10 1333.18 322.632 -3 10 -10 2474.10 405.125 -3 -10 -10 1621.71 360.972 3 -10 10 1126.46 306.780 -3 10 -10 1194.73 312.206 4 -10 10 2417.63 368.090 -4 10 -10 2417.49 408.622 4 -10 10 1866.16 397.079 -4 10 -10 2101.99 382.757 4 10 10 2479.20 443.844 -4 10 -10 2385.46 406.830 -4 -10 -10 2019.01 358.247 -4 10 -10 1429.17 324.390 -4 10 -10 2520.52 423.621 -4 -10 -10 2190.82 399.127 4 -10 10 2236.74 404.041 -4 10 -10 2355.66 406.507 -4 10 -10 2176.38 416.357 5 -10 10 251.662 168.895 -5 10 -10-71.8716 125.019 5 -10 10 59.1558 143.424 -5 10 -10 56.1967 131.192 5 10 10 108.583 211.434 -5 10 -10 330.596 256.704 -5 10 -10 204.124 155.476 -5 -10 -10 32.4832 129.446 -5 10 -10-51.9390 161.938 -5 10 -10 251.677 156.448 -5 10 -10 150.944 169.249 -5 -10 -10-4.44024 153.131 5 -10 10 133.279 143.905 6 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893.902 8 -10 10 10960.5 893.728 -8 10 -10 10645.8 880.274 8 -10 10 9697.30 815.297 9 -10 10 1772.29 375.137 -9 10 -10 1731.33 368.105 -9 10 -10 2030.89 399.179 -9 10 -10 1394.69 348.327 9 10 10 2957.07 524.403 9 -10 10 1756.15 372.854 -9 10 -10 1745.23 370.153 -9 -10 -10 1482.21 332.497 -9 -10 -10 2039.10 373.425 -9 10 -10 2094.78 392.068 -9 10 -10 2531.21 450.260 9 10 10 1918.55 345.603 -9 -10 -10 2239.44 409.626 9 -10 10 1950.03 400.013 -9 10 -10 2362.94 423.972 10 -10 10 282.946 252.552 10 -10 10-212.742 211.221 -10 10 -10 4.05990 126.146 -10 10 -10-34.0168 177.732 -10 10 -10 353.028 198.884 -10 -10 -10 494.256 225.008 -10 10 -10 133.744 158.696 -10 -10 -10 97.4023 117.845 -10 10 -10-75.8092 121.120 -10 10 -10 183.773 177.907 10 10 10 122.585 204.779 -10 -10 -10 269.663 159.551 10 -10 10 291.621 209.298 11 -10 10 4161.47 565.989 -11 10 -10 3325.08 506.634 -11 10 -10 3412.52 519.709 -11 10 -10 3476.93 523.119 -11 -10 -10 2556.06 440.867 -11 -10 -10 2369.40 433.779 -11 10 -10 3921.25 552.556 -11 10 -10 3426.01 535.188 11 10 10 3044.08 481.121 -11 -10 -10 3830.76 513.872 11 -10 10 3106.49 472.211 -11 10 -10 3690.21 531.062 11 -10 10 3244.62 510.662 -12 -10 -10-535.037 239.209 12 10 10 95.0487 172.318 -13 11 10 3220.22 506.663 -12 -11 10 309.668 220.226 -12 11 10 15.2518 166.081 -12 11 10-93.6017 212.830 12 -11 -10 206.481 214.481 -12 -11 10 218.657 188.547 -11 -11 10 3445.74 509.222 -11 11 10 3579.96 511.995 -11 11 10 3098.92 493.394 11 -11 -10 3331.49 509.829 -11 -11 10 4293.28 586.109 -10 -11 10 836.404 266.490 -10 11 10 664.768 247.941 -10 11 10 1222.81 308.938 10 -11 -10 1268.68 331.179 -10 -11 10 1264.23 354.155 -9 -11 10-100.913 166.342 9 11 -10 43.5599 165.195 -9 -11 10-206.119 206.043 9 11 -10-55.6784 192.453 -9 11 10 43.0800 168.212 9 -11 -10 416.117 250.411 -9 -11 10-268.308 219.729 9 11 -10-55.4358 136.338 8 -11 -10 2317.98 423.576 -8 -11 10 1926.03 394.887 8 11 -10 1921.22 390.590 -8 -11 10 1792.98 414.750 8 11 -10 1687.52 389.093 8 11 -10 1925.33 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748.025 221.813 0 8 12 1083.66 217.588 0 -8 12 933.597 228.830 0 -8 -12 967.416 257.973 0 8 -12 1085.13 279.940 1 -8 12 263.838 135.542 -1 8 -12 2.18452 130.352 -1 8 -12 15.8000 137.979 -1 8 -12-26.7886 111.206 1 8 12 88.0825 143.403 1 -8 12 709.590 281.692 -1 8 -12-575.977 206.662 -1 -8 -12 161.740 189.428 -1 8 -12-40.9766 127.307 -1 8 -12 31.0805 142.692 1 8 12 324.530 152.542 -1 -8 -12 119.131 156.623 1 -8 12 160.188 122.650 -1 -8 -12 288.658 118.538 -1 8 -12 68.1408 122.010 -2 8 -12 5376.53 573.226 -2 8 -12 5403.56 589.290 -2 8 -12 5797.02 593.751 2 8 12 5592.00 600.548 2 -8 12 4873.13 560.349 -2 -8 -12 5509.08 564.057 -2 8 -12 5766.31 592.218 -2 -8 -12 6043.17 499.869 -2 8 -12 5178.54 569.378 -2 8 -12 6447.87 604.051 2 -8 12 5654.24 520.833 2 8 12 6413.49 546.874 -2 -8 -12 5529.15 577.678 -2 8 -12 6539.13 628.660 2 -8 12 6033.10 497.450 -3 8 -12 1638.28 324.921 3 -8 12 2053.42 305.027 -3 8 -12 1951.93 349.314 -3 8 -12 1931.50 355.262 3 8 12 2081.03 388.637 3 -8 12 1945.59 370.985 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248.491 -8 8 -12 963.950 277.534 -8 8 -12 1010.85 286.126 -8 8 -12 1011.70 274.184 8 8 12 530.057 207.436 8 -8 12 317.970 202.052 -8 8 -12 764.406 266.142 -9 8 -12 581.680 213.527 9 -8 12 883.233 242.988 9 -8 12 680.554 236.489 -9 8 -12 1026.73 283.530 -9 8 -12 864.709 259.172 9 8 12 681.970 251.684 -9 -8 -12 650.699 222.555 -9 8 -12 298.104 191.174 -9 -8 -12 468.514 216.873 -9 8 -12 290.146 194.560 -9 8 -12 894.895 264.307 -9 8 -12 1232.28 291.472 9 8 12 502.514 207.655 9 -8 12 1288.89 312.488 -9 8 -12 1228.38 308.825 -10 8 -12 19.6434 170.031 10 -8 12 215.870 164.032 10 -8 12 182.625 181.382 -10 8 -12 151.550 170.701 10 8 12 122.250 145.672 -10 8 -12 269.804 188.420 -10 8 -12 122.332 144.093 -10 -8 -12-132.057 173.235 -10 -8 -12 284.545 196.474 -10 8 -12 444.513 216.742 -10 8 -12 445.896 231.438 -10 8 -12 55.3648 142.501 10 8 12-38.7034 141.674 10 -8 12 246.441 194.637 -10 8 -12 36.4677 180.994 -11 8 -12 948.669 288.619 11 -8 12 1014.88 290.299 11 -8 12 1005.54 296.091 -11 8 -12 644.748 239.922 11 8 12 958.023 319.898 -11 8 -12 949.503 286.635 -11 8 -12 1156.21 339.559 -11 -8 -12 682.456 246.033 -11 8 -12 817.873 267.876 -11 -8 -12 897.215 295.833 -11 8 -12 1607.83 357.671 -11 8 -12 826.965 261.874 -11 8 -12 756.012 238.326 11 8 12 711.752 273.477 11 -8 12 1097.09 299.014 12 -8 12 2229.52 398.410 -12 8 -12 1790.86 387.513 12 -8 12 2187.98 416.910 -12 8 -12 2388.20 438.215 12 8 12 2309.21 461.923 -12 8 -12 2559.30 438.110 -12 8 -12 3184.48 506.662 -12 -8 -12 2225.69 409.029 -12 -8 -12 1571.11 373.710 -12 8 -12 2584.72 468.980 -12 8 -12 2900.21 489.615 -12 8 -12 2328.56 414.821 12 8 12 2669.90 462.153 -12 8 -12 1990.21 416.257 13 -8 12 521.224 237.138 13 -8 12 516.738 236.285 -13 8 -12 402.779 211.429 -13 -8 -12 513.246 240.577 -13 8 -12 495.576 246.820 13 8 12 576.540 278.869 -14 8 -12 61.0839 150.963 -15 8 -12 48.6663 172.016 -16 9 12 848.331 296.874 -15 9 12 4778.96 609.348 -15 -9 12 5210.71 637.902 -15 9 12 4843.00 604.592 -15 -9 12 4985.67 592.148 15 -9 -12 4706.02 603.688 -14 9 12 4606.06 576.888 14 9 -12 4385.34 602.775 -14 -9 12 4477.13 576.301 -14 9 12 3794.61 524.734 -14 -9 12 3843.80 522.973 14 -9 -12 4483.55 588.785 13 9 -12 194.628 170.931 -13 -9 12 225.251 188.515 13 9 -12 36.0462 165.859 -13 9 12 443.789 205.739 13 9 -12 144.554 219.941 -13 -9 12 179.023 145.242 -13 9 12 93.4761 139.040 13 -9 -12 97.0319 175.069 -13 -9 12 248.354 177.887 13 -9 -12 141.948 216.397 13 9 -12 125.669 146.856 12 9 -12 3834.36 549.270 -12 -9 12 3493.45 542.057 12 9 -12 3592.73 522.918 -12 9 12 3114.30 460.564 12 9 -12 2786.36 463.615 -12 -9 12 3490.43 493.491 -12 9 12 3517.71 467.859 12 -9 -12 3753.94 535.936 12 -9 -12 2514.78 421.232 -12 -9 12 3922.52 528.880 12 -9 -12 2708.20 450.046 12 9 -12 3412.98 513.506 11 9 -12 1186.71 319.817 -11 -9 12 999.745 288.780 -11 9 12 1219.48 281.571 11 9 -12 818.169 260.772 11 9 -12 929.199 271.499 -11 -9 12 962.727 272.002 -11 9 12 1401.67 306.558 11 -9 -12 1612.66 360.970 11 -9 -12 1106.25 287.156 -11 -9 12 1374.61 334.599 11 -9 -12 1036.55 286.105 11 9 -12 768.174 268.286 10 9 -12 2464.64 429.958 -10 -9 12 2041.72 419.706 -10 9 12 2228.06 364.751 10 9 -12 2215.23 405.669 10 9 -12 2626.65 436.401 -10 -9 12 2264.92 392.328 -10 9 12 2533.96 390.071 10 -9 -12 3076.21 470.350 -10 -9 12 2126.60 408.426 10 -9 -12 2293.94 400.377 10 9 -12 2261.37 412.484 9 9 -12 1418.15 336.305 -9 9 12 2380.68 402.128 -9 -9 12 1556.70 360.284 -9 9 12 1364.78 271.259 9 9 -12 1490.56 346.163 9 9 -12 984.710 311.388 -9 -9 12 1955.68 348.038 -9 9 12 2340.61 362.700 9 -9 -12 1934.96 370.424 -9 -9 12 1288.47 316.002 9 -9 -12 1816.22 373.977 9 9 -12 1667.30 361.189 8 9 -12 607.579 247.211 8 9 -12 818.937 263.884 -8 9 12 581.832 216.314 -8 -9 12 432.392 233.605 -8 9 12 319.883 148.919 8 9 -12 472.430 197.877 8 9 -12 634.623 245.242 -8 -9 12 452.054 206.685 -8 9 12 323.483 149.407 8 -9 -12 456.513 235.769 -8 -9 12 231.269 231.207 8 -9 -12 191.959 159.029 7 9 -12 1085.82 267.817 7 9 -12 852.346 259.307 -7 9 12 767.026 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-23-30.8130 131.561 0 -2 23-81.1885 201.575 0 2 23-175.385 188.074 0 -2 23 5.88950 163.984 0 2 23 207.620 182.419 0 -2 -23-8.22215 126.562 0 2 -23 63.2285 167.673 0 2 -23-312.543 178.446 -1 2 -23 19.9942 136.617 -1 2 -23 346.473 197.088 -1 -2 -23 93.6630 163.338 -1 2 -23-108.118 168.245 -1 2 -23-72.9691 119.751 1 -2 23 44.0923 174.261 1 2 23 160.487 162.645 -1 -2 -23-122.979 187.226 -1 2 -23-176.640 179.052 -1 2 -23-204.477 177.280 -2 2 -23 600.883 219.877 -2 2 -23 851.986 260.517 -2 -2 -23 1484.31 349.970 -2 2 -23 909.381 264.453 -2 2 -23 999.821 281.484 2 -2 23 1175.81 310.306 2 2 23 951.108 287.930 -2 -2 -23 960.152 289.596 -2 2 -23 587.006 240.694 -2 2 -23 543.566 216.649 -3 2 -23 290.890 177.931 -3 2 -23 184.564 162.951 -3 -2 -23-18.1797 169.404 -3 2 -23 116.521 144.705 -3 2 -23-20.3317 150.916 -3 -2 -23-27.8230 144.426 -3 2 -23-140.710 174.158 -3 2 -23 94.6064 172.650 -4 2 -23 214.897 173.402 -4 2 -23-6.17576 150.464 -4 -2 -23 60.7020 148.073 -4 2 -23 324.641 214.952 -4 2 -23 114.709 145.461 -4 -2 -23 390.945 218.525 -4 2 -23 224.211 188.390 -4 2 -23-19.8721 148.945 -5 2 -23 46.2457 145.944 -5 2 -23-48.6159 146.936 -5 2 -23-100.753 159.691 -5 2 -23 275.536 180.629 -5 2 -23-72.0163 148.223 -11 -3 23 1147.59 321.688 -11 3 23 1061.03 282.536 10 3 -23 213.240 173.892 10 3 -23 304.551 188.379 -10 -3 23-102.961 178.329 10 3 -23 271.816 187.579 -10 -3 23 280.762 181.875 -10 3 23 605.438 247.713 9 3 -23 16.1066 123.299 9 3 -23-130.092 166.776 -9 -3 23-115.201 178.501 9 3 -23-14.9614 146.007 -9 -3 23 150.253 180.163 -9 3 23 58.4837 117.348 8 3 -23 308.238 173.546 8 3 -23 382.855 198.837 8 3 -23 500.853 216.649 -8 -3 23 885.377 286.021 -8 3 23-69.1641 135.998 7 3 -23 3614.07 483.461 7 3 -23 3187.23 450.690 7 3 -23 3663.21 489.812 -7 -3 23 3128.01 493.457 -7 3 23 3747.06 515.174 6 3 -23 1416.91 322.833 6 3 -23 1079.21 270.665 6 3 -23 814.851 259.117 -6 3 23 1036.74 314.290 -6 -3 23 1058.52 289.501 -6 3 23 1176.30 305.166 5 3 -23 1256.52 300.953 5 3 -23 965.257 262.885 5 3 -23 701.265 231.358 5 3 -23 1300.58 291.811 -5 3 23 555.316 241.916 -5 -3 23 721.391 279.416 -5 3 23 714.408 280.043 -5 -3 23 1165.91 323.073 -5 3 23 1357.72 339.421 5 -3 -23 1438.55 341.353 5 3 -23 1134.07 329.097 4 3 -23 2701.79 423.291 4 3 -23 2226.52 395.330 4 3 -23 3231.12 457.870 4 -3 -23 2426.23 429.890 4 3 -23 2476.37 410.527 -4 3 23 3324.00 507.737 -4 -3 23 2584.25 438.154 -4 -3 23 2869.70 499.966 -4 3 23 3227.49 489.557 4 -3 -23 2444.98 441.388 4 3 -23 3052.66 510.183 3 3 -23 1776.93 350.092 3 3 -23 1826.86 353.555 3 3 -23 2031.69 367.232 3 -3 -23 3040.96 477.117 3 3 -23 1933.41 368.358 -3 3 23 1787.59 386.933 -3 -3 23 2104.31 404.780 -3 -3 23 2413.04 464.760 -3 3 23 2566.60 451.634 3 -3 -23 1886.46 397.612 3 3 -23 2629.10 479.735 2 3 -23 62.5718 135.459 2 3 -23-122.390 156.186 2 3 -23 275.563 175.039 2 -3 -23 186.263 180.770 2 3 -23 233.912 168.160 -2 3 23 35.4897 183.711 -2 -3 23 15.8203 127.772 -2 3 23-46.3573 150.490 2 -3 -23 340.451 248.030 2 3 -23 173.905 196.677 2 3 -23-7.23750 127.198 1 3 -23 55.2403 162.383 1 3 -23 171.213 185.874 1 -3 -23 157.503 143.483 1 3 -23-308.194 194.216 1 3 -23-156.644 160.536 -1 -3 23-147.500 204.246 -1 3 23 283.025 227.052 -1 -3 23-315.094 209.714 -1 3 23-79.7056 156.663 1 -3 -23 86.7301 160.929 1 3 -23 105.308 146.722 1 3 -23 38.7389 143.949 0 3 -23 120.206 151.261 0 3 -23 23.9183 133.509 0 -3 -23 202.835 203.204 0 3 -23 163.602 125.054 0 3 -23-103.917 117.712 0 -3 23-103.159 124.664 0 3 23 62.2942 140.245 0 -3 -23 129.241 172.621 0 3 -23-65.2726 141.110 -1 3 -23 499.489 246.147 -1 3 -23 484.097 227.772 -1 -3 -23 130.794 163.793 -1 3 -23 14.1716 140.362 -1 3 -23 573.003 241.030 1 -3 23 384.784 198.500 1 3 23 660.540 258.665 -1 3 -23 129.589 170.077 -2 3 -23-70.1038 135.655 -2 3 -23-9.50101 124.559 -2 3 -23-188.944 191.139 -2 3 -23 85.2311 132.171 2 3 23-65.1463 167.363 -2 3 -23-134.282 147.323 -3 3 -23 41.7513 144.956 -3 3 -23 594.768 233.071 -3 3 -23 332.450 164.524 -3 3 -23 305.409 192.121 -3 3 -23 269.707 172.067 -4 3 -23 2143.40 402.272 -4 3 -23 2403.10 427.268 -4 3 -23 2155.78 410.105 -4 3 -23 2305.22 422.971 -4 3 -23 2254.67 419.555 12 4 -23 1356.89 334.816 -12 -4 23 1631.55 388.770 12 4 -23 445.088 231.813 12 4 -23 521.136 266.862 11 4 -23 1503.86 351.877 -11 -4 23 1442.69 354.229 11 4 -23 1893.76 388.023 -11 -4 23 1703.46 377.554 11 4 -23 1976.01 392.182 10 4 -23 1861.88 372.937 10 4 -23 2130.95 395.971 -10 -4 23 1629.12 367.862 10 4 -23 1682.35 358.927 -10 -4 23 1659.88 378.842 9 4 -23 118.990 180.683 9 4 -23 156.310 142.948 -9 -4 23 279.294 182.576 9 4 -23 383.575 214.214 -9 -4 23 666.295 269.170 8 4 -23 827.261 267.384 8 4 -23 608.901 237.415 8 4 -23 1242.83 306.070 -8 -4 23 386.240 203.223 7 4 -23 51.3197 127.052 7 4 -23 265.081 183.536 7 4 -23 0.28812 129.169 -7 -4 23 422.857 195.501 -7 4 23 84.8774 170.550 6 4 -23 570.764 232.921 6 4 -23 1103.24 285.706 6 4 -23 882.967 257.993 -6 -4 23 774.463 258.105 -6 4 23 1253.71 347.454 -6 4 23 979.104 268.890 5 4 -23-254.357 159.811 5 4 -23-4.92451 170.939 5 4 -23 201.574 193.563 5 4 -23 1.44150 148.828 -5 4 23-128.433 194.726 -5 -4 23 117.797 172.378 -5 4 23-264.411 207.378 4 4 -23 3228.41 481.570 4 4 -23 3538.49 504.187 4 4 -23 3166.32 475.848 4 4 -23 3763.90 514.046 -4 4 23 3646.68 539.616 -4 -4 23 3452.91 494.871 -4 4 23 3818.80 522.116 3 4 -23 488.336 214.672 3 4 -23 352.121 207.276 3 4 -23 545.629 247.892 3 4 -23 404.896 223.865 -3 4 23 349.462 221.299 -3 -4 23 417.562 220.419 -3 4 23 247.192 171.046 2 4 -23 143.549 154.960 2 4 -23 64.2076 124.179 2 4 -23 170.694 155.280 2 4 -23-116.694 171.065 -2 -4 23-74.4020 152.621 -2 4 23 106.853 136.436 1 4 -23 1834.85 378.067 1 4 -23 1523.89 353.896 1 4 -23 1824.65 380.707 1 4 -23 1665.26 364.394 -1 -4 23 1229.59 327.066 -1 -4 23 1579.88 347.336 -1 4 23 1369.40 334.962 1 4 -23 1922.16 392.499 0 4 -23 5302.35 627.927 0 4 -23 5107.05 613.221 0 4 -23 4697.42 592.496 0 4 -23 5386.09 622.289 0 -4 23 4336.68 576.203 0 4 23 4188.44 571.331 0 4 -23 5067.63 620.793 -1 4 -23 174.226 153.859 -1 4 -23 38.3456 119.456 -1 4 -23 65.4981 114.205 -1 4 -23 590.182 218.384 1 4 23 294.688 207.399 -1 4 -23 314.169 169.200 2 4 23 835.732 304.498 5 5 -23-44.9876 144.403 0 5 23 161.256 137.949 1 5 23 293.261 200.944 2 5 23 1679.59 362.620 -8 0 24 1197.63 337.292 -7 0 24 317.015 181.247 -6 0 24 1400.43 357.862 -6 0 24 1021.31 331.986 -5 0 24 1574.20 380.322 -5 0 24 1495.80 366.622 -4 0 24 80.4835 138.116 -4 0 24 674.850 290.955 -3 0 24 762.578 283.467 -3 0 24 575.162 244.613 1 0 -24 749.455 265.851 0 0 -24 7795.89 721.947 -1 0 -24-37.4441 127.740 -2 0 -24-124.456 182.546 -3 0 -24 2418.77 415.291 -4 0 -24 1270.41 319.656 -10 1 24 566.274 254.379 -9 1 24 48.3254 131.383 -8 1 24 206.631 179.048 -7 -1 24 481.689 243.165 -7 1 24 338.473 216.781 -6 -1 24 858.883 280.808 -6 1 24 385.069 211.153 -5 -1 24 227.788 196.048 -5 1 24-4.64529 130.984 -4 -1 24 3123.80 510.470 -4 1 24 3239.25 517.863 -3 -1 24 99.2141 191.899 -3 1 24 247.169 179.867 2 -1 -24 757.470 254.569 -2 1 24 835.161 287.378 1 -1 -24 209.070 169.097 0 -1 -24-263.948 212.450 -1 -1 -24-71.6816 131.377 -2 -1 -24 49.3961 131.386 -3 -1 -24 901.175 279.201 -11 2 24 724.062 262.872 -10 2 24 585.852 244.418 -9 2 24 60.5737 186.719 -8 -2 24 272.229 161.539 -8 2 24-97.6890 142.472 -7 -2 24 259.379 219.845 -7 2 24 343.660 183.835 -6 -2 24 488.287 237.507 -6 2 24 380.779 200.545 -5 -2 24 906.345 296.694 -5 2 24 588.540 231.584 -4 -2 24 944.000 315.729 -4 2 24 1029.65 307.016 3 -2 -24 4346.01 570.014 -3 -2 24 4174.16 570.949 -3 2 24 3839.03 556.721 2 -2 -24 3899.74 541.824 -2 -2 24 4647.60 604.917 -2 2 24 4469.16 609.971 1 2 -24 54.7746 113.768 1 2 -24 84.2597 129.370 1 -2 -24-25.3578 203.887 1 2 -24 149.754 166.608 1 2 -24 365.961 183.457 -1 2 24 226.404 215.354 1 2 -24 143.793 165.365 0 2 -24-75.9237 168.142 0 2 -24-89.3950 158.962 0 -2 -24 242.243 200.328 0 2 -24-192.127 167.324 0 2 -24-239.931 170.317 0 2 -24-27.4756 130.935 -1 2 -24 1810.25 359.773 -1 2 -24 1358.87 314.231 -1 2 -24 879.928 267.003 -1 2 -24 1622.16 345.996 -1 2 -24 1867.26 363.141 -2 2 -24 992.702 283.544 -2 2 -24 482.843 217.731 -2 2 -24 1064.24 288.141 -2 2 -24 490.508 206.489 -2 2 -24 984.569 290.432 -3 2 -24-172.195 190.057 -3 2 -24 135.260 195.612 -3 2 -24 357.335 217.678 -3 2 -24 382.655 229.046 -3 2 -24-92.3620 161.452 -10 3 24 1666.41 375.383 -9 3 24 1019.23 296.657 -8 -3 24 181.208 191.441 -8 3 24-22.2515 149.061 -7 -3 24 870.787 288.229 -7 3 24 1309.69 334.477 6 3 -24 679.559 229.163 6 3 -24 740.150 248.314 6 3 -24 714.688 231.510 -6 -3 24 1291.33 331.124 -6 3 24 548.034 221.812 5 3 -24 14.8417 148.490 5 3 -24 477.476 218.382 5 3 -24 483.935 195.772 5 3 -24 433.096 197.157 -5 -3 24 251.844 203.042 -5 3 24 237.398 167.226 4 3 -24 592.633 224.898 4 3 -24 1034.15 280.922 4 3 -24 1038.94 275.197 4 3 -24 991.952 269.764 -4 -3 24 485.822 224.617 -4 3 24 919.145 274.564 3 3 -24 49.4956 127.286 3 3 -24-69.7332 121.917 3 3 -24 205.518 183.222 3 3 -24 320.857 202.744 -3 -3 24 23.1541 153.003 -3 3 24 58.0982 147.861 2 3 -24 1630.65 355.416 2 3 -24 1890.05 377.371 2 3 -24 1885.44 371.994 2 3 -24 1306.61 316.895 -2 -3 24 1295.16 321.421 -2 3 24 2429.06 449.613 1 3 -24-170.475 158.488 1 3 -24 150.338 124.965 1 3 -24 235.797 154.603 1 3 -24 113.680 127.337 -1 -3 24 167.320 156.367 -1 3 24-221.995 193.871 1 3 -24 71.2813 152.565 0 3 -24 386.626 217.798 0 3 -24 443.619 211.082 0 3 -24 630.111 237.950 0 3 -24 490.281 222.105 0 3 -24 238.843 201.554 -1 3 -24 2439.80 441.754 -1 3 -24 3126.78 482.533 -1 3 -24 3085.00 484.786 -1 3 -24 3251.37 484.454 -1 3 -24 3397.67 504.665 9 4 -24 275.345 173.705 9 4 -24 479.310 220.678 -9 -4 24 238.681 206.874 9 4 -24 641.636 261.562 -9 -4 24 587.282 219.991 8 4 -24 33.4130 128.728 8 4 -24-160.155 176.259 8 4 -24 8.46346 141.004 -8 -4 24-248.648 195.927 7 4 -24 158.095 176.498 7 4 -24 85.2778 141.340 7 4 -24-58.1309 155.179 -7 -4 24 153.451 173.683 6 4 -24 147.933 148.219 6 4 -24 176.057 139.567 6 4 -24 23.7834 136.054 -6 -4 24-195.976 175.257 5 4 -24 420.363 206.194 5 4 -24 24.2626 143.086 5 4 -24 43.5459 115.517 5 4 -24 420.625 206.827 -5 -4 24 431.301 201.803 -5 4 24 561.914 252.628 4 4 -24 232.766 177.044 4 4 -24 485.821 246.140 4 4 -24 524.933 239.004 4 4 -24 346.055 223.356 -4 4 24 109.440 173.739 3 4 -24-41.8308 135.167 3 4 -24 160.050 138.648 3 4 -24 159.615 198.349 3 4 -24 267.201 183.775 -3 4 24 12.4912 157.051 -2 4 24 114.085 139.369 -1 4 24 984.324 295.973 1 0 -25 21.7469 122.133 0 0 -25 102.155 148.589 2 -1 -25 92.9305 150.473 0 0 0 0.00 0.00 TITL slaus in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 18.070958 9.532934 17.764238 90.0000 99.6133 90.0000 ZERR 9.00 0.000182 0.000094 0.000210 0.0000 0.0011 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H O Cl UNIT 108.00 117.00 18.00 45.00 TREF HKLF 4 END ; _shelx_hkl_checksum 40754 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 0.64397(8) 0.06200(16) 0.59499(10) 0.0169(3) Uani 1 1 d . . . . . H1 H 0.649868 0.069074 0.540136 0.020 Uiso 1 1 calc R U . . . C2 C 0.65315(9) 0.20950(19) 0.63032(13) 0.0306(4) Uani 1 1 d . . . . . H2A H 0.694676 0.207997 0.674391 0.037 Uiso 1 1 calc R U . . . H2B H 0.667099 0.275702 0.592093 0.037 Uiso 1 1 calc R U . . . C3 C 0.58236(9) 0.26223(17) 0.65684(10) 0.0197(3) Uani 1 1 d . . . . . H3 H 0.578073 0.211695 0.705255 0.024 Uiso 1 1 calc R U . . . C4 C 0.58685(9) 0.41899(18) 0.67512(12) 0.0294(4) Uani 1 1 d . . . . . H4A H 0.594784 0.471530 0.629065 0.035 Uiso 1 1 calc R U . . . H4B H 0.630501 0.436700 0.715681 0.035 Uiso 1 1 calc R U . . . C5 C 0.51546(10) 0.47292(19) 0.70155(10) 0.0278(4) Uani 1 1 d . . . . . H5A H 0.512516 0.434049 0.752649 0.033 Uiso 1 1 calc R U . . . H5B H 0.517737 0.576418 0.705916 0.033 Uiso 1 1 calc R U . . . C6 C 0.44674(8) 0.43163(16) 0.64675(8) 0.0153(3) Uani 1 1 d . . . . . C7 C 0.44153(8) 0.27719(16) 0.62856(9) 0.0163(3) Uani 1 1 d . . . . . H7A H 0.396671 0.259281 0.589485 0.020 Uiso 1 1 calc R U . . . H7B H 0.435841 0.223940 0.675094 0.020 Uiso 1 1 calc R U . . . C8 C 0.51221(8) 0.22631(14) 0.59873(8) 0.0110(3) Uani 1 1 d . . . . . C9 C 0.50780(8) 0.06803(15) 0.59198(8) 0.0119(3) Uani 1 1 d . . . . . C10 C 0.70227(8) -0.04257(17) 0.63463(9) 0.0180(3) Uani 1 1 d . . . . . C11 C 0.39360(8) 0.52223(15) 0.61786(8) 0.0143(3) Uani 1 1 d . . . . . C12 C 0.51343(10) 0.28648(16) 0.51905(9) 0.0191(3) Uani 1 1 d . . . . . H12A H 0.467483 0.259014 0.484745 0.029 Uiso 1 1 calc R U . . . H12B H 0.557168 0.249913 0.499385 0.029 Uiso 1 1 calc R U . . . H12C H 0.516428 0.389026 0.522010 0.029 Uiso 1 1 calc R U . . . O1 O 0.57299(6) -0.00453(11) 0.59868(7) 0.0168(2) Uani 1 1 d . . . . . O2 O 0.45063(6) 0.00121(11) 0.58304(7) 0.0197(2) Uani 1 1 d . . . . . Cl1 Cl 0.69149(2) -0.20800(4) 0.58851(3) 0.02650(9) Uani 1 1 d . . . . . Cl2 Cl 0.69309(3) -0.06541(7) 0.73158(3) 0.03676(12) Uani 1 1 d . . . . . Cl3 Cl 0.79325(2) 0.02104(4) 0.62849(3) 0.02334(9) Uani 1 1 d . . . . . Cl4 Cl 0.39513(2) 0.69915(4) 0.63813(2) 0.01916(8) Uani 1 1 d . . . . . Cl5 Cl 0.31339(2) 0.47544(4) 0.55522(3) 0.02852(10) Uani 1 1 d . . . . . C1' C 0.14437(8) 0.05878(15) 0.57761(9) 0.0143(3) Uani 1 1 d . . . . . H1' H 0.148829 0.041069 0.523065 0.017 Uiso 1 1 calc R U . . . C2' C 0.15425(8) 0.21743(16) 0.59197(10) 0.0177(3) Uani 1 1 d . . . . . H2'1 H 0.205491 0.235240 0.619984 0.021 Uiso 1 1 calc R U . . . H2'2 H 0.149318 0.266383 0.542233 0.021 Uiso 1 1 calc R U . . . C3' C 0.09743(8) 0.27848(15) 0.63742(8) 0.0133(3) Uani 1 1 d . . . . . H3' H 0.108576 0.239058 0.690266 0.016 Uiso 1 1 calc R U . . . C4' C 0.10375(8) 0.43834(16) 0.64359(10) 0.0178(3) Uani 1 1 d . . . . . H4'1 H 0.096962 0.479182 0.591650 0.021 Uiso 1 1 calc R U . . . H4'2 H 0.154633 0.463625 0.670036 0.021 Uiso 1 1 calc R U . . . C5' C 0.04504(9) 0.50157(17) 0.68740(9) 0.0189(3) Uani 1 1 d . . . . . H5'1 H 0.057839 0.476488 0.742112 0.023 Uiso 1 1 calc R U . . . H5'2 H 0.045745 0.605103 0.683240 0.023 Uiso 1 1 calc R U . . . C6' C -0.03242(8) 0.44775(15) 0.65575(8) 0.0140(3) Uani 1 1 d . . . . . C7' C -0.03824(8) 0.29047(15) 0.65077(9) 0.0156(3) Uani 1 1 d . . . . . H7'1 H -0.089920 0.263370 0.627580 0.019 Uiso 1 1 calc R U . . . H7'2 H -0.027370 0.249613 0.702684 0.019 Uiso 1 1 calc R U . . . C8' C 0.01781(8) 0.23280(14) 0.60205(8) 0.0110(3) Uani 1 1 d . . . . . C9' C 0.01317(8) 0.07442(15) 0.60173(8) 0.0133(3) Uani 1 1 d . . . . . C10' C 0.20433(8) -0.03101(16) 0.62746(9) 0.0171(3) Uani 1 1 d . . . . . C11' C -0.09099(9) 0.53102(16) 0.63353(9) 0.0155(3) Uani 1 1 d . . . . . C12' C -0.00559(9) 0.27863(16) 0.51827(8) 0.0180(3) Uani 1 1 d . . . . . H12D H 0.025799 0.230465 0.486392 0.027 Uiso 1 1 calc R U . . . H12E H 0.000925 0.380266 0.514275 0.027 Uiso 1 1 calc R U . . . H12F H -0.058360 0.254309 0.500854 0.027 Uiso 1 1 calc R U . . . O1' O 0.07393(6) -0.00009(11) 0.59021(7) 0.0180(2) Uani 1 1 d . . . . . O2' O -0.04206(6) 0.00900(11) 0.60902(7) 0.0216(2) Uani 1 1 d . . . . . Cl1' Cl 0.18996(2) -0.21184(4) 0.60665(3) 0.03412(12) Uani 1 1 d . . . . . Cl2' Cl 0.20273(2) -0.00417(6) 0.72576(2) 0.03137(11) Uani 1 1 d . . . . . Cl3' Cl 0.29388(2) 0.01505(4) 0.60733(2) 0.02004(8) Uani 1 1 d . . . . . Cl4' Cl -0.08923(2) 0.71139(4) 0.64253(2) 0.01934(8) Uani 1 1 d . . . . . Cl5' Cl -0.17868(2) 0.47037(4) 0.59157(2) 0.02348(9) 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 0.0088(6) 0.0142(7) 0.0270(8) -0.0036(6) 0.0013(6) 0.0003(5) C2 0.0121(7) 0.0204(8) 0.0575(13) -0.0160(8) 0.0003(7) -0.0002(6) C3 0.0144(7) 0.0184(7) 0.0234(8) -0.0089(6) -0.0050(6) 0.0038(6) C4 0.0166(8) 0.0204(8) 0.0463(11) -0.0193(8) -0.0096(7) 0.0041(6) C5 0.0277(9) 0.0247(9) 0.0265(9) -0.0143(7) -0.0090(7) 0.0114(7) C6 0.0183(7) 0.0152(7) 0.0132(6) -0.0020(5) 0.0047(5) 0.0034(5) C7 0.0160(7) 0.0130(7) 0.0210(7) 0.0024(6) 0.0065(6) 0.0034(5) C8 0.0106(6) 0.0107(6) 0.0115(6) -0.0011(5) 0.0010(5) 0.0002(5) C9 0.0116(6) 0.0121(6) 0.0123(6) 0.0002(5) 0.0026(5) 0.0021(5) C10 0.0119(6) 0.0225(8) 0.0193(7) -0.0033(6) 0.0019(5) 0.0023(6) C11 0.0164(7) 0.0125(6) 0.0147(7) -0.0012(5) 0.0048(5) 0.0013(5) C12 0.0299(8) 0.0133(7) 0.0153(7) 0.0014(6) 0.0071(6) 0.0010(6) O1 0.0086(5) 0.0127(5) 0.0287(6) -0.0039(4) 0.0014(4) 0.0005(4) O2 0.0123(5) 0.0127(5) 0.0347(6) -0.0008(5) 0.0057(4) -0.0011(4) Cl1 0.01760(18) 0.01685(18) 0.0440(3) -0.00572(17) 0.00200(16) 0.00501(14) Cl2 0.0226(2) 0.0681(4) 0.0190(2) 0.0022(2) 0.00166(16) 0.0038(2) Cl3 0.00953(15) 0.0258(2) 0.0345(2) -0.00551(16) 0.00325(14) 0.00135(14) Cl4 0.02697(19) 0.01238(16) 0.01904(17) -0.00166(13) 0.00645(14) 0.00454(13) Cl5 0.01867(18) 0.02098(19) 0.0417(2) -0.00656(17) -0.00722(17) 0.00650(15) C1' 0.0090(6) 0.0138(7) 0.0200(7) -0.0013(5) 0.0028(5) 0.0010(5) C2' 0.0126(6) 0.0128(7) 0.0290(8) -0.0014(6) 0.0075(6) -0.0010(5) C3' 0.0109(6) 0.0123(6) 0.0161(7) -0.0021(5) 0.0002(5) 0.0002(5) C4' 0.0126(6) 0.0124(7) 0.0273(8) -0.0041(6) 0.0004(6) -0.0022(5) C5' 0.0183(7) 0.0160(7) 0.0216(7) -0.0059(6) 0.0008(6) 0.0009(6) C6' 0.0162(7) 0.0125(6) 0.0145(7) -0.0009(5) 0.0056(5) 0.0009(5) C7' 0.0148(7) 0.0113(6) 0.0220(7) 0.0020(5) 0.0066(6) 0.0021(5) C8' 0.0101(6) 0.0086(6) 0.0140(6) 0.0002(5) 0.0010(5) -0.0002(5) C9' 0.0115(6) 0.0108(6) 0.0170(7) 0.0000(5) 0.0009(5) 0.0016(5) C10' 0.0116(6) 0.0153(7) 0.0246(8) 0.0006(6) 0.0038(6) 0.0007(5) C11' 0.0182(7) 0.0131(7) 0.0158(7) -0.0007(5) 0.0048(5) 0.0016(5) C12' 0.0238(8) 0.0139(7) 0.0148(7) 0.0003(5) -0.0017(6) -0.0001(6) O1' 0.0083(5) 0.0113(5) 0.0340(6) -0.0027(4) 0.0031(4) -0.0004(4) O2' 0.0139(5) 0.0124(5) 0.0400(7) 0.0000(5) 0.0088(5) -0.0021(4) Cl1' 0.01494(18) 0.01350(18) 0.0712(3) 0.00024(19) -0.00072(19) 0.00236(14) Cl2' 0.0226(2) 0.0503(3) 0.0215(2) 0.00949(19) 0.00465(15) 0.00833(19) Cl3' 0.00962(15) 0.02010(18) 0.0313(2) -0.00076(15) 0.00595(13) 0.00106(13) Cl4' 0.02666(19) 0.01160(16) 0.02000(17) -0.00114(13) 0.00458(14) 0.00500(13) Cl5' 0.01545(17) 0.02128(19) 0.0321(2) -0.00376(16) -0.00083(15) 0.00378(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 O1 C1 C10 103.96(12) . . ? O1 C1 C2 114.82(13) . . ? C10 C1 C2 112.83(13) . . ? C3 C2 C1 112.94(13) . . ? C2 C3 C4 111.81(14) . . ? C2 C3 C8 111.17(13) . . ? C4 C3 C8 111.70(13) . . ? C3 C4 C5 112.05(15) . . ? C6 C5 C4 111.20(13) . . ? C11 C6 C5 123.20(14) . . ? C11 C6 C7 122.47(14) . . ? C5 C6 C7 114.31(13) . . ? C6 C7 C8 110.84(12) . . ? C9 C8 C12 107.98(12) . . ? C9 C8 C3 107.60(12) . . ? C12 C8 C3 113.62(13) . . ? C9 C8 C7 107.76(12) . . ? C12 C8 C7 109.93(12) . . ? C3 C8 C7 109.74(12) . . ? O2 C9 O1 117.20(13) . . ? O2 C9 C8 124.85(13) . . ? O1 C9 C8 117.92(12) . . ? C1 C10 Cl2 110.96(11) . . ? C1 C10 Cl3 108.82(11) . . ? Cl2 C10 Cl3 109.90(8) . . ? C1 C10 Cl1 110.61(10) . . ? Cl2 C10 Cl1 108.61(9) . . ? Cl3 C10 Cl1 107.90(8) . . ? C6 C11 Cl4 124.73(12) . . ? C6 C11 Cl5 123.63(12) . . ? Cl4 C11 Cl5 111.64(8) . . ? C9 O1 C1 122.59(12) . . ? O1' C1' C2' 115.94(12) . . ? O1' C1' C10' 104.42(12) . . ? C2' C1' C10' 113.58(12) . . ? C3' C2' C1' 113.17(12) . . ? C2' C3' C4' 111.68(12) . . ? C2' C3' C8' 110.10(12) . . ? C4' C3' C8' 111.45(12) . . ? C3' C4' C5' 112.11(13) . . ? C6' C5' C4' 110.68(12) . . ? C11' C6' C7' 122.23(14) . . ? C11' C6' C5' 123.42(14) . . ? C7' C6' C5' 114.35(13) . . ? C6' C7' C8' 110.04(12) . . ? C9' C8' C3' 109.43(11) . . ? C9' C8' C7' 108.51(12) . . ? C3' C8' C7' 109.18(12) . . ? C9' C8' C12' 105.86(12) . . ? C3' C8' C12' 113.73(12) . . ? C7' C8' C12' 109.97(12) . . ? O2' C9' O1' 116.99(13) . . ? O2' C9' C8' 124.34(13) . . ? O1' C9' C8' 118.64(12) . . ? C1' C10' Cl2' 111.18(11) . . ? C1' C10' Cl3' 108.98(11) . . ? Cl2' C10' Cl3' 109.24(8) . . ? C1' C10' Cl1' 110.87(10) . . ? Cl2' C10' Cl1' 108.68(9) . . ? Cl3' C10' Cl1' 107.82(8) . . ? C6' C11' Cl4' 124.46(12) . . ? C6' C11' Cl5' 123.63(12) . . ? Cl4' C11' Cl5' 111.91(8) . . ? C9' O1' C1' 125.40(11) . . ? 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 O1 1.4422(17) . ? C1 C10 1.534(2) . ? C1 C2 1.537(2) . ? C2 C3 1.521(2) . ? C3 C4 1.529(2) . ? C3 C8 1.5339(19) . ? C4 C5 1.533(2) . ? C5 C6 1.497(2) . ? C6 C11 1.329(2) . ? C6 C7 1.507(2) . ? C7 C8 1.541(2) . ? C8 C9 1.5147(19) . ? C8 C12 1.531(2) . ? C9 O2 1.2014(18) . ? C9 O1 1.3542(17) . ? C10 Cl2 1.7712(17) . ? C10 Cl3 1.7727(16) . ? C10 Cl1 1.7728(17) . ? C11 Cl4 1.7238(15) . ? C11 Cl5 1.7319(15) . ? C1' O1' 1.4424(17) . ? C1' C2' 1.539(2) . ? C1' C10' 1.540(2) . ? C2' C3' 1.524(2) . ? C3' C4' 1.531(2) . ? C3' C8' 1.5338(19) . ? C4' C5' 1.540(2) . ? C5' C6' 1.509(2) . ? C6' C11' 1.329(2) . ? C6' C7' 1.505(2) . ? C7' C8' 1.539(2) . ? C8' C9' 1.5121(19) . ? C8' C12' 1.541(2) . ? C9' O2' 1.2020(18) . ? C9' O1' 1.3517(17) . ? C10' Cl2' 1.7700(17) . ? C10' Cl3' 1.7700(15) . ? C10' Cl1' 1.7729(16) . ? C11' Cl4' 1.7267(15) . ? C11' Cl5' 1.7340(16) . ? 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 O1 C1 C2 C3 -4.8(2) . . . . ? C10 C1 C2 C3 -123.65(16) . . . . ? C1 C2 C3 C4 -167.38(16) . . . . ? C1 C2 C3 C8 -41.8(2) . . . . ? C2 C3 C4 C5 179.74(16) . . . . ? C8 C3 C4 C5 54.4(2) . . . . ? C3 C4 C5 C6 -51.3(2) . . . . ? C4 C5 C6 C11 -129.11(17) . . . . ? C4 C5 C6 C7 52.6(2) . . . . ? C11 C6 C7 C8 126.40(15) . . . . ? C5 C6 C7 C8 -55.26(18) . . . . ? C2 C3 C8 C9 61.28(17) . . . . ? C4 C3 C8 C9 -173.06(14) . . . . ? C2 C3 C8 C12 -58.21(18) . . . . ? C4 C3 C8 C12 67.45(18) . . . . ? C2 C3 C8 C7 178.28(14) . . . . ? C4 C3 C8 C7 -56.07(18) . . . . ? C6 C7 C8 C9 172.44(12) . . . . ? C6 C7 C8 C12 -70.10(15) . . . . ? C6 C7 C8 C3 55.55(16) . . . . ? C12 C8 C9 O2 -93.30(18) . . . . ? C3 C8 C9 O2 143.68(15) . . . . ? C7 C8 C9 O2 25.4(2) . . . . ? C12 C8 C9 O1 88.74(15) . . . . ? C3 C8 C9 O1 -34.29(17) . . . . ? C7 C8 C9 O1 -152.56(13) . . . . ? O1 C1 C10 Cl2 -62.88(14) . . . . ? C2 C1 C10 Cl2 62.15(16) . . . . ? O1 C1 C10 Cl3 176.09(10) . . . . ? C2 C1 C10 Cl3 -58.88(16) . . . . ? O1 C1 C10 Cl1 57.72(14) . . . . ? C2 C1 C10 Cl1 -177.25(12) . . . . ? C5 C6 C11 Cl4 0.2(2) . . . . ? C7 C6 C11 Cl4 178.40(11) . . . . ? C5 C6 C11 Cl5 -179.29(13) . . . . ? C7 C6 C11 Cl5 -1.1(2) . . . . ? O2 C9 O1 C1 167.86(14) . . . . ? C8 C9 O1 C1 -14.0(2) . . . . ? C10 C1 O1 C9 159.01(13) . . . . ? C2 C1 O1 C9 35.3(2) . . . . ? O1' C1' C2' C3' 15.69(19) . . . . ? C10' C1' C2' C3' -105.28(15) . . . . ? C1' C2' C3' C4' -174.20(13) . . . . ? C1' C2' C3' C8' -49.84(17) . . . . ? C2' C3' C4' C5' 178.33(12) . . . . ? C8' C3' C4' C5' 54.73(17) . . . . ? C3' C4' C5' C6' -50.46(18) . . . . ? C4' C5' C6' C11' -127.10(16) . . . . ? C4' C5' C6' C7' 52.57(18) . . . . ? C11' C6' C7' C8' 122.73(15) . . . . ? C5' C6' C7' C8' -56.94(17) . . . . ? C2' C3' C8' C9' 59.02(16) . . . . ? C4' C3' C8' C9' -176.49(13) . . . . ? C2' C3' C8' C7' 177.65(12) . . . . ? C4' C3' C8' C7' -57.86(16) . . . . ? C2' C3' C8' C12' -59.12(16) . . . . ? C4' C3' C8' C12' 65.37(16) . . . . ? C6' C7' C8' C9' 177.13(12) . . . . ? C6' C7' C8' C3' 57.92(15) . . . . ? C6' C7' C8' C12' -67.51(15) . . . . ? C3' C8' C9' O2' 147.18(15) . . . . ? C7' C8' C9' O2' 28.1(2) . . . . ? C12' C8' C9' O2' -89.88(18) . . . . ? C3' C8' C9' O1' -34.94(18) . . . . ? C7' C8' C9' O1' -153.99(13) . . . . ? C12' C8' C9' O1' 88.00(15) . . . . ? O1' C1' C10' Cl2' -67.41(13) . . . . ? C2' C1' C10' Cl2' 59.83(15) . . . . ? O1' C1' C10' Cl3' 172.13(10) . . . . ? C2' C1' C10' Cl3' -60.63(15) . . . . ? O1' C1' C10' Cl1' 53.61(14) . . . . ? C2' C1' C10' Cl1' -179.16(11) . . . . ? C7' C6' C11' Cl4' 176.32(12) . . . . ? C5' C6' C11' Cl4' -4.0(2) . . . . ? C7' C6' C11' Cl5' -3.9(2) . . . . ? C5' C6' C11' Cl5' 175.79(12) . . . . ? O2' C9' O1' C1' 177.78(14) . . . . ? C8' C9' O1' C1' -0.3(2) . . . . ? C2' C1' O1' C9' 10.7(2) . . . . ? C10' C1' O1' C9' 136.47(14) . . . . ?