#------------------------------------------------------------------------------ #$Date: 2024-06-20 01:22:26 +0300 (Thu, 20 Jun 2024) $ #$Revision: 292468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571949.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_1571949 loop_ _publ_author_name 'Arnold, Robert' 'Saska, Jan' 'Mesquita-Ribeiro, Raquel' 'Dajas-Bailador, Federico' 'Lewis, William' 'Taylor, Laurence John' 'Argent, Stephen' 'Shaoh, Huiling' 'Houk, K. N.' 'Denton, Ross Matthew' _publ_section_title ; Total Synthesis, Biological Evaluation and Biosynthetic Re-Evaluation of Illicium-Derived Neolignans ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03232B _journal_year 2024 _chemical_formula_moiety 'C19 H19 Br O3' _chemical_formula_sum 'C19 H19 Br O3' _chemical_formula_weight 375.25 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2018-02-22 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2024-01-23 deposited with the CCDC. 2024-06-13 downloaded from the CCDC. ; _cell_angle_alpha 90.265(4) _cell_angle_beta 105.787(4) _cell_angle_gamma 106.880(4) _cell_formula_units_Z 2 _cell_length_a 8.0674(3) _cell_length_b 10.0413(5) _cell_length_c 11.4509(5) _cell_measurement_reflns_used 10446 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 74.4480 _cell_measurement_theta_min 4.0290 _cell_volume 850.63(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 10.3613 _diffrn_detector_type 'Agilent Diffraction Atlas detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -50.00 34.00 1.00 2.50 -- -38.50 38.00 -60.00 84 2 \w -109.00 -12.00 1.00 2.50 -- -38.50 -57.00 0.00 97 3 \w -65.00 32.00 1.00 2.50 -- -38.50 57.00 150.00 97 4 \w 1.00 83.00 1.00 2.50 -- 43.32 -99.00-150.00 82 5 \w 1.00 83.00 1.00 2.50 -- 43.32 -99.00-120.00 82 6 \w 35.00 98.00 1.00 10.00 -- 106.13 -45.00 -60.00 63 7 \w 31.00 91.00 1.00 10.00 -- 106.13 -30.00-120.00 60 8 \w 32.00 138.00 1.00 10.00 -- 106.13 -77.00 120.00 106 9 \w 31.00 91.00 1.00 10.00 -- 106.13 -30.00 90.00 60 10 \w 25.00 109.00 1.00 10.00 -- 106.13 -95.00 60.00 84 11 \w 25.00 109.00 1.00 10.00 -- 106.13 -95.00-120.00 84 12 \w 35.00 98.00 1.00 10.00 -- 106.13 -45.00-150.00 63 13 \w 35.00 121.00 1.00 10.00 -- 106.13-125.00 -60.00 86 14 \w 31.00 91.00 1.00 10.00 -- 106.13 -30.00 120.00 60 15 \w 35.00 98.00 1.00 10.00 -- 106.13 -45.00 30.00 63 16 \w 31.00 91.00 1.00 10.00 -- 106.13 -30.00 60.00 60 17 \w 25.00 109.00 1.00 10.00 -- 106.13 -95.00 -30.00 84 18 \w 19.00 178.00 1.00 10.00 -- 106.13 0.00 -90.00 159 19 \w -50.00 34.00 1.00 2.50 -- -38.50 38.00 60.00 84 20 \w 17.00 113.00 1.00 2.50 -- 43.32 57.00 -90.00 96 21 \w 12.00 117.00 1.00 2.50 -- 43.32 77.00 150.00 105 22 \w 17.00 113.00 1.00 2.50 -- 43.32 57.00 60.00 96 23 \w 12.00 117.00 1.00 2.50 -- 43.32 77.00 -60.00 105 24 \w 82.00 178.00 1.00 10.00 -- 106.13 30.00 -30.00 96 25 \w 75.00 178.00 1.00 10.00 -- 106.13 77.00 150.00 103 26 \w 61.00 178.00 1.00 10.00 -- 106.13 15.00 90.00 117 27 \w 82.00 177.00 1.00 10.00 -- 106.13 45.00 -90.00 95 28 \w 79.00 176.00 1.00 10.00 -- 106.13 61.00-150.00 97 29 \w 79.00 176.00 1.00 10.00 -- 106.13 61.00 0.00 97 30 \w 75.00 178.00 1.00 10.00 -- 106.13 77.00 60.00 103 31 \w 79.00 176.00 1.00 10.00 -- 106.13 61.00 -30.00 97 32 \w 75.00 178.00 1.00 10.00 -- 106.13 77.00-180.00 103 33 \w 79.00 176.00 1.00 10.00 -- 106.13 61.00 120.00 97 34 \w 12.00 67.00 1.00 2.50 -- 43.32 77.00 90.00 55 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1419749000 _diffrn_orient_matrix_UB_12 0.1015917000 _diffrn_orient_matrix_UB_13 -0.0504568000 _diffrn_orient_matrix_UB_21 0.1122728000 _diffrn_orient_matrix_UB_22 -0.1028947000 _diffrn_orient_matrix_UB_23 0.0193747000 _diffrn_orient_matrix_UB_31 -0.1029666000 _diffrn_orient_matrix_UB_32 -0.0707896000 _diffrn_orient_matrix_UB_33 -0.1295689000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0173 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 16326 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.626 _diffrn_reflns_theta_min 4.029 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 3.393 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.465 _exptl_crystal_description needle _exptl_crystal_F_000 384 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: diethyl ether, petroleum ether' _exptl_crystal_size_max 0.391 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.028 _refine_diff_density_max 0.362 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.057 _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 209 _refine_ls_number_reflns 3423 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0234 _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^)+(0.0326P)^2^+0.5214P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.0617 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3321 _reflns_number_total 3423 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03232b2.cif _cod_data_source_block 30 _cod_database_code 1571949 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'C19 H19 Br O3' _chemical_oxdiff_usercomment 'REARDG #17455 SN-1272 IN FOMBLIN FILM ON A MICROMOUNT FOR REA/RD' _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 0.911 _shelx_estimated_absorpt_t_min 0.350 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.13 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C2(H2) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C12(H12A,H12B), C20(H20A,H20B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C8(H8), C14(H14), C15(H15), C17(H17), C18(H18), C21(H21) 2.d X=CH2 refined with riding coordinates: C22(H22A,H22B) 2.e Idealised Me refined as rotating group: C13(H13A,H13B,H13C) ; _shelx_res_file ; TITL reardg.res created by SHELXL-2018/1 at 23:12:45 on 22-Feb-2018 CELL 1.54184 8.067362 10.041331 11.450902 90.2651 105.7869 106.8797 ZERR 2 0.00034 0.000473 0.000468 0.0036 0.0038 0.004 LATT 1 SFAC C H O Br UNIT 38 38 6 2 L.S. 12 PLAN 20 SIZE 0.028 0.06 0.391 TEMP -153 bond $h conf htab fmap 2 acta OMIT -1 -5 13 REM REM REM WGHT 0.032600 0.521400 FVAR 6.61047 O1 3 0.646060 0.719967 0.325098 11.00000 0.01366 0.02166 = 0.02460 0.00495 0.00667 0.00499 C2 1 0.711927 0.611534 0.382437 11.00000 0.01691 0.02110 = 0.02314 0.00357 0.00863 0.00627 AFIX 13 H2 2 0.622112 0.555360 0.422530 11.00000 -1.20000 AFIX 0 C3 1 0.889748 0.673074 0.478450 11.00000 0.01788 0.02230 = 0.01937 0.00344 0.00818 0.00755 AFIX 23 H3A 2 0.931040 0.596371 0.518083 11.00000 -1.20000 H3B 2 0.872002 0.730773 0.541622 11.00000 -1.20000 AFIX 0 C4 1 1.038462 0.764767 0.425272 11.00000 0.01356 0.01812 = 0.01742 0.00010 0.00385 0.00485 C5 1 0.954257 0.850290 0.329547 11.00000 0.01551 0.01905 = 0.01557 -0.00079 0.00372 0.00555 C6 1 1.065652 0.958807 0.284762 11.00000 0.01395 0.02370 = 0.01894 0.00029 0.00279 0.00373 AFIX 43 H6 2 1.192995 0.978380 0.315012 11.00000 -1.20000 AFIX 0 C7 1 0.996388 1.039330 0.197237 11.00000 0.01916 0.02120 = 0.01931 0.00052 0.00439 0.00292 C8 1 0.809178 1.011934 0.156013 11.00000 0.02136 0.02260 = 0.01649 0.00141 0.00193 0.00714 AFIX 43 H8 2 0.758331 1.066725 0.097681 11.00000 -1.20000 AFIX 0 C9 1 0.697841 0.904654 0.200413 11.00000 0.01393 0.02293 = 0.01717 -0.00128 0.00148 0.00593 C10 1 0.767017 0.821862 0.285913 11.00000 0.01509 0.01790 = 0.01680 -0.00152 0.00475 0.00403 O11 3 0.731406 0.523152 0.296002 11.00000 0.01655 0.02265 = 0.02614 -0.00228 0.00697 0.00353 C12 1 0.564067 0.456978 0.203728 11.00000 0.02009 0.03047 = 0.02704 -0.00344 0.00446 0.00193 AFIX 23 H12A 2 0.525105 0.527406 0.152114 11.00000 -1.20000 H12B 2 0.468336 0.411958 0.242267 11.00000 -1.20000 AFIX 0 C13 1 0.594609 0.349660 0.127695 11.00000 0.03497 0.04089 = 0.03596 -0.01242 0.01052 0.00324 AFIX 137 H13A 2 0.482816 0.304494 0.063292 11.00000 -1.50000 H13B 2 0.630358 0.279257 0.179192 11.00000 -1.50000 H13C 2 0.690641 0.394994 0.090840 11.00000 -1.50000 AFIX 0 C14 1 1.178536 0.860597 0.529786 11.00000 0.02067 0.02128 = 0.01858 0.00111 0.00492 0.00704 AFIX 43 H14 2 1.145207 0.930105 0.566371 11.00000 -1.20000 AFIX 0 C15 1 1.346434 0.854297 0.574398 11.00000 0.01895 0.02650 = 0.01828 -0.00255 0.00057 0.00417 AFIX 43 H15 2 1.427142 0.918324 0.641106 11.00000 -1.20000 AFIX 0 C16 1 1.409873 0.750699 0.522932 11.00000 0.01599 0.03156 = 0.01956 0.00413 0.00588 0.00744 C17 1 1.285969 0.667660 0.410579 11.00000 0.01822 0.02564 = 0.02182 0.00250 0.00890 0.00838 AFIX 43 H17 2 1.326847 0.607698 0.368502 11.00000 -1.20000 AFIX 0 C18 1 1.118083 0.673855 0.365892 11.00000 0.01650 0.01977 = 0.01756 0.00132 0.00644 0.00498 AFIX 43 H18 2 1.044315 0.618023 0.292629 11.00000 -1.20000 AFIX 0 O19 3 1.556737 0.733931 0.571951 11.00000 0.01899 0.05403 = 0.02461 0.00047 0.00303 0.01705 C20 1 1.124124 1.150146 0.146435 11.00000 0.02083 0.03005 = 0.02547 0.00708 0.00464 0.00194 AFIX 23 H20A 2 1.239208 1.189244 0.211469 11.00000 -1.20000 H20B 2 1.151055 1.104854 0.079828 11.00000 -1.20000 AFIX 0 C21 1 1.054727 1.267453 0.098709 11.00000 0.03051 0.02461 = 0.03385 0.00414 0.01041 0.00343 AFIX 43 H21 2 1.020261 1.318853 0.152868 11.00000 -1.20000 AFIX 0 C22 1 1.037636 1.305115 -0.012616 11.00000 0.04465 0.03120 = 0.03471 0.01007 0.00589 0.00960 AFIX 93 H22A 2 1.070700 1.256232 -0.069412 11.00000 -1.20000 H22B 2 0.992216 1.381228 -0.036317 11.00000 -1.20000 AFIX 0 BR23 4 0.443347 0.869407 0.145962 11.00000 0.01430 0.03118 = 0.02145 0.00149 0.00105 0.00808 HKLF 4 REM REM R1 = 0.0234 for 3321 Fo > 4sig(Fo) and 0.0242 for all 3423 data REM 209 parameters refined using 0 restraints END WGHT 0.0326 0.5214 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y+2, -z HTAB C8 Br23_$1 EQIV $2 -x+2, -y+1, -z+1 HTAB C12 O19_$2 EQIV $3 -x+2, -y+2, -z+1 HTAB C15 Br23_$3 REM Highest difference peak 0.362, deepest hole -0.315, 1-sigma level 0.057 Q1 1 0.4170 0.9345 0.1000 11.00000 0.05 0.36 Q2 1 0.9928 0.8071 0.3757 11.00000 0.05 0.35 Q3 1 1.0744 0.7166 0.4009 11.00000 0.05 0.34 Q4 1 1.3487 0.7262 0.4649 11.00000 0.05 0.30 Q5 1 0.8063 0.6457 0.4237 11.00000 0.05 0.30 Q6 1 0.7463 0.9611 0.1700 11.00000 0.05 0.30 Q7 1 0.8629 0.8306 0.3071 11.00000 0.05 0.29 Q8 1 1.0003 0.8844 0.2925 11.00000 0.05 0.28 Q9 1 1.1139 0.8170 0.4770 11.00000 0.05 0.28 Q10 1 0.7270 0.8595 0.2388 11.00000 0.05 0.28 Q11 1 0.4685 0.7945 0.2044 11.00000 0.05 0.27 Q12 1 1.3736 0.7962 0.5421 11.00000 0.05 0.27 Q13 1 1.0254 1.0012 0.2450 11.00000 0.05 0.26 Q14 1 1.2735 0.8639 0.5334 11.00000 0.05 0.26 Q15 1 1.2500 0.8234 0.5731 11.00000 0.05 0.25 Q16 1 0.3877 0.7379 0.1391 11.00000 0.05 0.24 Q17 1 0.9567 0.7237 0.4405 11.00000 0.05 0.24 Q18 1 1.0521 1.0855 0.1768 11.00000 0.05 0.24 Q19 1 0.5017 1.0013 0.1599 11.00000 0.05 0.23 Q20 1 0.6969 0.7615 0.3029 11.00000 0.05 0.23 ; _shelx_res_checksum 45887 _shelx_hkl_file ; 0 0 -1 18256.9 288.176 3 0 0 1 18623.2 332.817 2 0 0 -1 19005.0 236.298 1 0 0 2 22696.5 514.555 2 0 0 -2 21561.8 448.632 3 0 0 -2 23267.2 371.202 1 0 0 -2 24128.9 511.928 19 0 0 2 22275.3 386.816 20 0 0 3 190738. 1350.72 20 0 0 -3 191224. 1307.88 1 0 0 3 192693. 1862.10 2 0 0 3 189928. 1861.43 23 0 0 4 149659. 1920.38 2 0 0 -4 156488. 1986.74 19 0 0 4 149916. 1353.47 20 0 0 -4 155255. 2153.74 4 0 0 -4 151428. 1325.70 1 0 0 4 150081. 1915.25 23 0 0 -4 160713. 2150.64 5 0 0 5 2913.90 332.268 23 0 0 -5 3184.89 206.109 1 0 0 5 2882.37 311.911 2 0 0 5 3140.88 209.433 20 0 0 -5 2608.21 320.097 5 0 0 -5 3044.05 344.884 19 0 0 -5 2707.75 347.484 4 0 0 -6 72922.0 1820.78 19 0 0 6 76581.7 1731.85 2 0 0 -6 79514.8 2042.35 5 0 0 6 71175.4 1710.03 23 0 0 7 144910. 2538.69 2 0 0 7 141715. 2715.00 23 0 0 -8 132.587 74.8138 17 0 0 -8 181.344 128.619 11 0 0 -8 138.400 85.8011 13 0 0 8 108.892 166.585 23 0 0 -9 3634.27 337.862 11 0 0 -9 3401.62 303.997 13 0 0 9 2765.42 581.017 22 0 0 -9 3427.24 312.118 17 0 0 -10 7482.91 476.301 17 0 0 -10 8033.81 482.855 11 0 0 -10 7389.12 444.817 13 0 0 -11 16575.4 687.160 17 0 0 -11 17907.1 699.394 11 0 0 -11 16795.3 631.400 13 0 0 -12 354.850 159.321 11 0 0 -12 349.590 127.939 17 0 0 -12 394.069 111.682 13 0 0 -13 4673.24 281.833 17 0 1 -13 8451.61 376.749 17 0 1 -12 13273.4 565.664 17 0 1 -12 11915.3 440.791 13 0 1 -11 320.881 194.003 11 0 1 -11 479.045 165.216 17 0 1 -11 179.856 93.6156 13 0 1 -10 33185.3 870.277 13 0 1 -10 33928.9 976.750 11 0 1 -10 34141.6 1004.93 17 0 1 -9 23462.9 789.595 17 0 1 -9 24036.4 796.831 11 0 1 -9 24026.8 718.652 13 0 1 -8 28292.4 804.627 17 0 1 -8 26409.2 814.423 30 0 -1 8 28688.1 1446.11 23 0 1 -8 27517.7 729.376 13 0 1 -8 30239.0 808.618 11 0 -1 7 17580.3 1024.80 23 0 -1 7 18096.2 913.055 2 0 -1 6 43519.1 1410.50 23 0 1 -6 40819.6 1460.82 19 0 -1 6 44974.0 1307.29 2 0 1 -6 43532.0 1530.85 5 0 1 -5 91906.0 1910.43 19 0 -1 5 86807.2 1657.09 2 0 1 -5 86454.5 1336.03 1 0 -1 5 86127.6 1747.09 23 0 -1 5 91520.5 1194.13 20 0 1 -5 93366.2 1907.50 5 0 1 -4 87349.6 1226.74 1 0 -1 4 90435.2 1499.62 2 0 1 -4 92802.3 1709.83 19 0 1 -4 95006.0 1678.07 5 0 -1 4 92079.8 1109.64 20 0 -1 4 88284.7 1556.29 23 0 -1 3 118127. 1566.22 23 0 1 -3 124104. 1609.93 5 0 1 -3 122800. 1717.52 19 0 -1 3 119270. 1155.28 20 0 -1 3 114039. 1494.70 2 0 -1 2 2901.40 209.545 2 0 1 -2 2924.21 202.521 5 0 -1 2 2684.67 158.483 20 0 1 -2 2586.27 229.398 19 0 1 -2 2679.10 208.023 21 0 -1 1 22626.8 430.063 20 0 -1 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15 0 -7 3 19091.3 560.055 16 0 -7 3 19517.7 653.024 31 0 7 -3 19948.5 655.104 26 0 7 -3 20005.8 1332.00 21 0 7 -3 19639.9 676.574 33 0 -7 3 20523.5 630.480 18 0 -7 3 19098.7 1176.38 3 0 -7 3 21375.5 1542.00 23 0 -7 3 19585.4 621.305 27 0 7 -2 33156.2 792.814 26 0 -7 2 32296.1 718.121 15 0 7 -2 32823.3 1754.65 21 0 -7 2 34805.8 1901.81 23 0 7 -2 31722.7 863.490 33 0 -7 2 32796.1 716.858 16 0 -7 2 31850.5 1532.89 3 0 -7 2 33845.2 801.117 27 0 -7 2 31981.0 773.799 18 0 -7 2 31952.0 791.463 24 0 -7 1 22509.0 1574.95 23 0 7 -1 23465.3 637.770 26 0 -7 1 22522.2 638.042 24 0 7 -1 22505.9 1477.42 21 0 7 -1 22903.5 716.505 33 0 -7 1 22110.0 589.215 16 0 -7 1 21037.7 635.137 18 0 -7 1 23421.9 675.876 27 0 -7 1 23172.8 606.718 15 0 -7 1 21908.3 1279.46 3 0 -7 0 74064.9 2363.79 3 0 -7 0 74035.8 1079.98 15 0 7 0 74343.7 1257.87 33 0 -7 0 69305.2 1097.58 18 0 7 0 71554.3 2652.00 21 0 -7 0 72031.4 1066.89 16 0 -7 0 75475.1 1227.51 27 0 -7 -1 987.283 168.600 27 0 7 1 695.510 337.280 21 0 -7 -1 887.454 124.860 16 0 -7 -1 810.692 311.080 3 0 -7 -1 1026.13 140.877 15 0 -7 -2 44525.6 824.661 10 0 -7 -2 45116.0 996.094 27 0 7 2 46112.0 2213.86 21 0 -7 -2 47891.2 880.948 15 0 -7 -2 46347.2 1955.60 3 0 -7 -2 46392.7 854.818 16 0 7 3 25737.2 1698.75 21 0 -7 -3 26658.9 778.787 27 0 -7 -3 24033.3 638.961 10 0 -7 -3 25789.8 1501.32 3 0 -7 -3 25038.2 628.539 16 0 -7 -3 25790.9 659.132 15 0 -7 -4 96.2724 79.4290 15 0 7 4-51.5936 205.692 21 0 -7 -4 126.963 121.739 8 0 -7 -4 122.558 118.893 3 0 -7 -4 133.251 116.866 10 0 -7 -5 11406.8 436.543 15 0 -7 -5 11502.8 477.894 10 0 -7 -6 7609.59 396.673 10 0 -7 -6 8076.12 493.740 8 0 -7 -7 13723.9 590.615 8 0 -7 -7 14145.4 521.387 10 0 -7 -8 222.319 138.630 10 0 -7 -8 237.036 106.694 8 0 -7 -9 721.594 147.659 10 0 -7 -10 28259.7 497.813 10 0 8 -11 4522.52 208.656 6 0 -8 11 5090.11 235.738 31 0 -8 10 20948.3 592.857 31 0 8 -10 22223.6 517.230 7 0 8 -10 20839.2 500.545 17 0 8 -10 20986.9 518.450 33 0 8 -9 5438.65 286.163 18 0 8 -9 6353.81 352.947 33 0 -8 9 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0 8 -3 21401.5 707.538 26 0 8 -3 20461.3 728.512 25 0 -8 3 19162.7 1265.36 3 0 8 -2 275.736 182.155 21 0 -8 2 291.539 214.854 3 0 8 -2 388.333 139.966 33 0 -8 2 765.958 142.019 16 0 -8 2 267.484 234.441 23 0 -8 2 564.029 161.360 27 0 -8 2 559.935 140.794 24 0 -8 2 613.783 128.300 15 0 8 -2 380.232 124.191 26 0 -8 1 2735.48 230.999 16 0 -8 1 3038.83 291.205 27 0 -8 1 2201.46 436.999 3 0 8 -1 2895.85 289.962 33 0 -8 1 2691.56 235.615 15 0 8 -1 2977.21 259.326 26 0 -8 1 3258.02 267.644 24 0 8 -1 2757.86 571.293 21 0 8 0 38654.3 2133.76 21 0 -8 0 41442.0 869.983 16 0 -8 0 42085.1 880.237 15 0 8 0 41460.5 1009.51 33 0 -8 0 43000.7 1016.32 27 0 -8 0 39843.8 1886.82 3 0 8 1 4067.01 704.547 21 0 -8 -1 5417.01 328.440 15 0 8 1 4755.24 346.121 33 0 -8 -1 4912.19 362.001 27 0 -8 -1 5102.15 315.814 16 0 -8 -1 5248.70 708.673 3 0 8 2 516.568 129.789 33 0 -8 -2 600.756 173.453 27 0 -8 -2 367.089 112.163 15 0 -8 -2 615.331 134.382 16 0 -8 -2 486.657 115.518 10 0 -8 -3 54352.0 965.364 16 0 -8 -3 53595.4 984.210 15 0 -8 -3 55025.2 1324.25 8 0 -8 -3 55405.9 1170.51 27 0 -8 -4 5461.41 295.992 16 0 -8 -4 5135.61 314.357 10 0 -8 -4 5558.60 319.680 15 0 -8 -4 6028.75 386.030 27 0 -8 -4 5760.24 445.846 8 0 -8 -5 13334.1 465.315 15 0 -8 -5 14029.7 501.677 10 0 -8 -5 14124.3 665.550 8 0 -8 -6 2705.92 301.570 8 0 -8 -6 3363.42 216.213 15 0 -8 -6 3166.89 250.116 10 0 -8 -7 16451.5 598.071 8 0 -8 -7 19574.2 553.861 10 0 -8 -8 2358.60 197.367 10 0 -8 -9 586.825 162.386 10 0 9 -10 6181.30 239.936 6 0 -9 9 4999.03 273.174 31 0 9 -9 5153.30 263.301 33 0 9 -9 4727.78 215.265 17 0 -9 9 4817.93 248.142 24 0 9 -9 5062.55 239.106 7 0 9 -8 3256.97 235.438 18 0 -9 8 3709.41 273.371 31 0 9 -8 3709.31 231.726 17 0 9 -8 3396.37 226.064 7 0 -9 8 3622.58 253.833 24 0 9 -8 3872.43 270.822 33 0 9 -7 1780.43 221.004 33 0 9 -7 1716.30 180.823 7 0 -9 7 1400.65 205.226 24 0 -9 7 1623.68 207.930 31 0 -9 6 15591.2 521.804 27 0 -9 6 16110.3 594.111 24 0 9 -6 15349.3 620.144 33 0 -9 6 14973.7 476.041 9 0 -9 6 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514.429 27 0 -9 -1 10418.2 456.160 15 0 -9 -2 7676.35 503.993 8 0 9 2 7733.99 425.780 33 0 -9 -2 8623.71 480.736 27 0 -9 -2 8056.59 387.113 16 0 -9 -2 8914.27 418.248 15 0 -9 -3 14808.7 505.011 10 0 -9 -3 14737.5 509.012 9 0 -9 -3 15150.7 501.241 16 0 9 3 15033.6 560.240 33 0 -9 -3 15957.8 533.285 15 0 -9 -3 14928.5 614.339 27 0 -9 -4 264.818 156.673 8 0 -9 -4 415.528 119.249 15 0 -9 -4 257.026 74.1676 16 0 9 4 325.538 97.8803 33 0 -9 -4 332.031 174.720 10 0 -9 -5 3635.27 267.890 10 0 -9 -5 4173.57 328.504 8 0 -9 -5 3926.03 233.078 15 0 -9 -6 1616.26 195.498 8 0 -9 -6 1134.13 204.747 10 0 -9 -7 133.841 78.5589 8 0 10 -8 2011.58 126.725 7 0 10 -8 2081.77 154.841 33 0 -10 8 1883.99 155.045 24 0 -10 7 369.126 96.4585 24 0 10 -7 372.540 72.4113 7 0 10 -7 536.919 107.717 33 0 10 -6 1559.52 132.530 7 0 10 -6 2011.71 204.857 33 0 -10 6 1664.82 141.228 9 0 -10 6 1614.24 150.736 27 0 -10 6 1316.61 179.760 24 0 10 -6 1338.76 181.922 18 0 10 -6 963.504 135.863 17 0 -10 5 10239.7 395.579 9 0 -10 5 10133.3 359.060 16 0 -10 5 9916.43 442.781 24 0 10 -5 11419.1 491.844 33 0 -10 5 10372.7 434.160 27 0 -10 4 16625.1 538.615 9 0 -10 4 16669.2 558.586 24 0 -10 4 16331.4 496.040 16 0 -10 4 17869.6 594.897 27 0 10 -4 15827.5 592.760 33 0 -10 3 547.623 121.030 16 0 -10 3 333.029 90.4363 24 0 10 -3 573.436 153.841 33 0 -10 3 552.578 161.833 27 0 -10 3 452.833 135.481 9 0 -10 2 10736.3 427.682 24 0 10 -2 11675.8 494.343 25 0 -10 2 11697.5 457.567 16 0 -10 2 11471.5 520.533 27 0 10 -2 10574.9 498.663 33 0 -10 1 1850.51 240.394 27 0 10 -1 911.642 208.709 25 0 10 -1 1398.38 201.950 33 0 -10 1 1737.51 198.932 16 0 -10 1 1062.94 194.599 8 0 10 0 11933.7 516.632 33 0 -10 0 14451.5 591.586 27 0 -10 0 12329.7 494.503 9 0 -10 0 13094.0 499.941 15 0 -10 0 12061.8 544.067 8 0 -10 0 13462.5 492.199 16 0 -10 -1 6255.59 392.390 27 0 -10 -1 5341.91 375.593 8 0 10 1 5298.75 334.607 33 0 -10 -1 5544.40 328.809 9 0 -10 -1 6179.23 335.511 16 0 -10 -1 6331.24 345.752 15 0 -10 -2 8688.63 453.336 27 0 -10 -2 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4714.28 258.149 16 2 -8 -4 13240.0 484.839 15 2 -8 -4 13384.6 453.028 10 -2 8 4 13099.8 1191.42 21 2 -8 -3 29330.8 722.796 15 2 -8 -3 28945.6 744.813 27 2 -8 -3 29982.1 1704.01 3 -2 8 3 27009.8 1679.96 21 2 -8 -2 9559.04 416.463 15 2 -8 -2 10148.9 446.179 27 2 -8 -2 9440.47 382.123 18 2 -8 -2 11220.8 1031.72 3 -2 8 2 10701.3 1038.77 21 -2 8 1 4693.49 702.253 21 -2 8 1 4401.59 591.947 1 2 -8 -1 5325.30 694.716 3 2 -8 -1 5338.65 309.735 15 -2 8 1 4791.81 295.697 26 2 -8 -1 4930.69 295.363 18 2 -8 -1 5460.50 337.115 27 -2 8 0 13795.0 532.716 26 2 -8 0 15883.2 513.117 15 2 -8 0 16396.0 565.359 27 2 -8 0 16523.3 1190.06 3 -2 8 0 13518.8 1045.62 1 2 -8 0 15710.6 520.685 18 2 -8 1 17002.8 1168.94 3 -2 8 -1 15613.9 558.913 26 2 -8 1 16508.2 550.126 18 -2 8 -1 15321.3 1145.87 1 2 -8 1 16624.8 568.658 27 2 -8 1 17167.9 1327.82 23 2 -8 1 15975.4 532.881 24 2 -8 1 15889.0 501.836 15 -2 8 -1 17553.6 650.217 33 2 -8 2 2172.37 219.756 27 -2 8 -2 2511.07 487.058 1 2 -8 2 1988.22 206.222 18 2 -8 2 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1908.32 21 2 -6 1 15253.3 998.070 20 2 -6 1 15637.0 948.945 3 2 -6 1 14730.3 993.262 23 -2 6 -1 16076.2 880.895 21 2 -6 2 35195.1 1512.89 20 2 -6 2 34660.8 1581.70 23 2 -6 2 35636.1 1384.38 3 -2 6 -2 32034.4 1519.16 1 2 -6 3 61979.9 1738.41 3 2 -6 3 58759.2 1998.28 20 -2 6 -3 57641.4 2098.16 1 2 -6 3 61871.3 2238.96 23 2 -6 4 1717.88 166.912 18 -2 6 -4 2059.07 189.549 30 2 -6 4 1414.99 458.394 23 -2 6 -4 1626.84 378.701 1 -2 6 -4 1650.21 192.390 33 -2 6 -4 1802.57 177.284 12 -2 6 -4 1831.61 187.410 26 2 -6 4 1750.59 405.336 20 -2 6 -5 24931.0 678.171 12 -2 6 -5 25573.0 679.759 30 2 -6 5 26134.7 651.390 18 -2 6 -5 23413.2 686.568 26 -2 6 -5 24253.3 722.313 33 2 -6 5 25025.8 1625.89 23 -2 6 -5 24409.6 1466.97 1 2 -6 5 22525.8 1318.89 20 2 -6 5 24084.8 606.849 27 -2 6 -6 5385.82 342.156 30 -2 6 -6 4928.61 330.381 12 -2 6 -6 4830.59 325.951 26 2 -6 6 4730.17 307.186 18 2 -6 6 5558.66 855.932 23 -2 6 -6 5503.09 316.634 7 -2 6 -6 5471.01 718.523 1 -2 6 -7 10383.8 488.376 30 -2 6 -7 9896.48 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519.802 110.314 26 4 -11 4 635.378 97.7266 24 -4 11 -4 536.194 75.2695 7 4 -11 5 19782.3 419.237 24 -4 11 -5 15627.1 327.896 7 4 -10 -8 14954.8 308.158 15 4 -10 -7 13282.3 357.967 15 4 -10 -6 3838.07 228.607 15 4 -10 -6 2349.24 207.643 8 4 -10 -5 11855.7 371.959 16 4 -10 -5 13617.6 436.402 15 4 -10 -4 7751.13 346.321 15 4 -10 -3 10283.3 420.073 27 4 -10 -3 9662.67 408.967 15 -4 10 2 5008.88 278.656 30 -4 10 2 4770.15 342.884 33 4 -10 -2 4762.25 300.678 27 4 -10 -2 5114.10 283.951 15 -4 10 2 4718.97 276.584 26 4 -10 -2 4677.90 273.753 18 -4 10 1 3942.73 311.434 33 -4 10 1 3976.55 247.462 30 4 -10 -1 3807.66 287.034 27 4 -10 -1 3384.69 224.754 15 -4 10 1 3397.59 254.430 26 4 -10 -1 3807.89 260.408 18 -4 10 0 12548.5 524.514 33 4 -10 0 12654.8 497.749 27 4 -10 0 12339.0 415.076 15 -4 10 0 11088.7 478.813 26 -4 10 0 12598.5 436.790 30 4 -10 0 12618.2 465.896 18 -4 10 -1 7620.63 399.891 33 4 -10 1 7250.23 349.658 24 -4 10 -1 7515.48 338.165 30 4 -10 1 7730.02 404.290 27 -4 10 -1 7500.27 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33 -4 9 -1 3852.10 277.643 30 4 -9 1 3832.20 288.885 27 -4 9 -1 3991.61 304.299 26 -4 9 -2 6721.63 382.325 33 4 -9 2 6479.29 355.336 18 4 -9 2 6917.55 375.216 27 -4 9 -2 5898.85 373.526 26 -4 9 -2 6613.49 354.117 30 4 -9 3 42247.0 894.248 18 -4 9 -3 43971.0 888.995 30 4 -9 3 41356.6 716.807 16 4 -9 3 43742.0 891.743 27 -4 9 -3 43855.3 963.826 26 -4 9 -4 11533.9 449.545 30 4 -9 4 11300.5 451.208 27 -4 9 -4 13697.5 527.781 26 4 -9 4 13339.1 507.771 24 -4 9 -4 11492.7 410.871 12 -4 9 -4 12494.5 438.659 7 4 -9 4 12268.5 471.306 18 -4 9 -5 6295.20 328.503 30 4 -9 5 5609.75 301.478 27 -4 9 -5 5725.50 345.462 26 4 -9 5 6151.58 364.177 24 -4 9 -5 6128.83 300.863 12 -4 9 -5 6687.87 320.553 7 4 -9 5 5534.47 307.217 18 -4 9 -6 11262.8 407.734 30 -4 9 -6 10152.3 416.655 26 4 -9 6 12339.0 439.202 24 -4 9 -6 11107.4 388.273 12 -4 9 -6 11379.4 394.070 7 -4 9 -7 10743.5 366.170 30 4 -9 7 9356.90 350.197 31 -4 9 -7 11183.3 399.849 17 -4 9 -7 10372.7 340.655 12 4 -9 7 9620.37 364.161 24 -4 9 -7 11161.4 362.378 7 -4 9 -8 2369.80 154.001 17 -4 9 -8 2395.71 152.256 30 4 -9 8 1987.23 139.754 24 -4 9 -8 1907.57 131.384 7 4 -8 -10 19578.0 429.408 10 4 -8 -9 122.884 78.6057 10 4 -8 -9 129.124 56.6299 15 -4 8 8 6213.96 381.773 30 4 -8 -8 5707.12 290.837 10 4 -8 -8 5828.35 290.157 15 4 -8 -7 258.178 96.3085 10 -4 8 7 155.355 182.193 30 4 -8 -7 305.482 110.005 15 4 -8 -7 306.381 124.593 28 4 -8 -6 21003.7 684.862 28 4 -8 -6 19928.8 535.381 10 4 -8 -6 19282.5 587.691 15 4 -8 -5 14614.1 605.268 28 4 -8 -5 15027.6 526.373 15 -4 8 5 14805.8 677.504 30 -4 8 4 7686.05 501.505 30 4 -8 -4 7719.14 444.992 28 4 -8 -4 7811.47 388.101 15 -4 8 4 7500.52 374.211 26 4 -8 -3 438.773 118.325 18 4 -8 -3 364.295 110.127 28 4 -8 -3 293.325 88.6175 27 4 -8 -3 479.956 121.844 15 -4 8 3 264.251 95.0617 26 -4 8 3 550.912 195.753 30 4 -8 -2 4580.18 314.464 18 -4 8 2 4627.20 370.853 30 4 -8 -2 4435.39 701.089 3 4 -8 -2 5278.71 310.067 27 4 -8 -2 4706.02 290.842 15 -4 8 2 4406.22 308.921 26 4 -8 -2 4541.13 332.418 28 4 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26 -4 8 -5 24915.3 679.588 12 -4 8 -5 25523.5 704.888 30 4 -8 5 24390.9 652.464 18 4 -8 6 114.742 57.5312 18 -4 8 -6 116.963 101.289 30 4 -8 6 52.0722 67.2612 27 -4 8 -6 76.1330 69.1471 26 -4 8 -6 96.3536 98.6384 12 -4 8 -6 26.6096 104.845 7 -4 8 -7 596.392 119.889 30 -4 8 -7 613.132 130.219 17 -4 8 -7 451.247 99.3672 26 4 -8 7 493.393 116.199 24 -4 8 -7 549.756 119.684 12 -4 8 -7 569.343 121.926 7 -4 8 -8 29559.7 636.527 30 -4 8 -8 30455.7 652.862 17 -4 8 -8 30025.6 592.140 12 -4 8 -8 30267.5 575.854 7 4 -8 9 6.93860 43.0605 31 -4 8 -9 118.538 55.2470 30 -4 8 -9 172.682 58.0313 12 -4 7 11 6279.63 290.713 30 4 -7 -11 12105.8 345.818 10 4 -7 -10 3047.43 212.254 10 4 -7 -9 3405.14 240.272 10 4 -7 -9 3348.91 213.528 15 4 -7 -8 7089.39 409.124 32 4 -7 -8 6590.97 390.082 28 4 -7 -8 6396.25 325.879 15 4 -7 -8 7495.77 357.773 10 4 -7 -7 6359.76 390.165 32 4 -7 -7 6399.63 332.913 10 4 -7 -7 6688.07 352.780 15 4 -7 -7 6791.74 400.303 28 4 -7 -6 631.741 124.294 10 4 -7 -6 849.435 175.502 28 4 -7 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8667.36 395.745 15 4 -6 -8 10097.2 481.541 32 4 -6 -7 26740.8 768.478 32 4 -6 -7 24740.3 800.005 28 4 -6 -7 26559.0 671.568 10 -4 6 7 24972.5 1611.08 22 -4 6 7 27150.9 1892.64 34 4 -6 -6 5988.65 402.621 32 4 -6 -6 8455.91 360.478 10 4 -6 -6 8070.06 454.015 28 4 -6 -6 8180.12 869.912 3 -4 6 6 7700.17 975.702 2 -4 6 6 7703.99 874.545 22 -4 6 6 7393.75 992.139 34 4 -6 -5 4151.75 281.461 32 4 -6 -5 3824.61 239.653 10 4 -6 -5 3505.73 542.261 3 4 -6 -5 4463.18 304.451 28 -4 6 5 3885.62 250.746 26 -4 6 5 4264.50 659.027 22 4 -6 -5 4431.62 565.444 19 -4 6 5 3680.88 706.864 34 4 -6 -4 24456.0 577.789 18 -4 6 4 23149.3 1639.55 34 4 -6 -4 26284.5 1452.36 3 -4 6 4 23672.8 616.547 26 4 -6 -4 25199.8 644.469 32 -4 6 4 23057.7 1440.52 22 4 -6 -4 24010.1 651.897 28 4 -6 -3 53817.5 868.636 18 -4 6 3 50913.9 1152.81 30 4 -6 -3 58054.8 2046.27 3 4 -6 -3 55653.5 927.556 28 -4 6 3 52354.2 918.504 26 -4 6 3 54250.6 2177.82 22 4 -6 -3 54920.9 1855.58 20 4 -6 -3 53725.1 889.033 32 -4 6 3 47199.7 2256.20 34 -4 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48407.8 1748.99 5 -4 4 -5 50127.2 969.536 8 4 -4 5 51225.2 835.719 27 -4 4 -5 51174.5 992.844 30 -4 4 -5 52920.7 2120.91 1 -4 4 -5 53616.5 976.116 13 4 -4 5 53438.6 2177.70 23 -4 4 -5 49469.2 1001.20 12 -4 4 -5 45611.1 885.524 11 4 -4 5 48957.7 1862.18 20 -4 4 -6 1178.74 176.742 30 -4 4 -6 1502.61 194.558 17 -4 4 -6 1379.95 179.106 8 -4 4 -6 1344.01 174.786 13 4 -4 6 1099.10 331.088 23 -4 4 -6 1433.67 201.287 12 -4 4 -6 1494.87 184.607 11 4 -4 6 1151.03 288.063 20 -4 4 -7 302.470 120.527 30 -4 4 -7 504.388 118.582 17 -4 4 -7 623.788 125.534 13 -4 4 -7 645.157 157.964 12 -4 4 -7 444.906 96.8334 7 -4 4 -7 290.746 121.046 11 -4 4 -8 25199.2 750.846 30 -4 4 -8 25897.1 675.737 13 -4 4 -8 25342.8 683.870 12 -4 4 -8 25865.1 701.147 11 -4 4 -9 7510.04 387.555 30 -4 4 -9 8290.00 369.337 17 -4 4 -9 7385.49 336.238 12 -4 4 -9 7786.66 344.502 13 -4 4 -9 7569.02 357.618 11 -4 4 -10 205.651 70.0864 13 -4 4 -10 194.697 83.1162 11 4 -3 -13 1729.26 129.310 10 4 -3 -13 1484.26 174.195 17 4 -3 -12 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13085.6 469.082 18 5 -7 -4 14361.7 556.157 28 5 -7 -4 12508.5 1131.08 3 -5 7 4 13601.3 513.273 26 -5 7 4 12957.3 1280.49 2 -5 7 4 13169.9 1183.11 22 5 -7 -4 13281.3 1113.47 19 5 -7 -3 448.632 109.468 18 -5 7 3 320.299 187.928 30 5 -7 -3 376.066 97.0567 28 -5 7 3 305.710 192.050 2 5 -7 -3 496.020 114.929 27 5 -7 -3 895.576 309.588 3 -5 7 3 478.231 129.833 26 -5 7 3 690.826 323.584 22 5 -7 -2 2888.43 239.080 18 -5 7 2 2123.65 313.029 30 5 -7 -2 2618.36 237.938 28 5 -7 -2 3277.83 252.844 27 5 -7 -2 2005.09 211.952 15 -5 7 2 2634.98 238.349 26 -5 7 2 3078.31 600.356 22 5 -7 -2 2617.97 450.770 20 5 -7 -1 20178.0 615.339 18 -5 7 1 19917.3 723.552 30 5 -7 -1 19230.8 586.760 28 -5 7 1 18874.5 1329.78 1 5 -7 -1 19822.0 592.072 27 5 -7 -1 19899.6 549.140 15 -5 7 1 19409.6 637.088 26 5 -7 -1 18601.7 1288.05 20 5 -7 0 33859.6 813.350 18 -5 7 0 34132.3 908.686 30 -5 7 0 36356.8 1946.79 1 5 -7 0 35135.3 754.599 28 5 -7 0 35371.0 800.555 27 -5 7 0 35166.5 866.290 26 5 -7 0 33496.8 1712.28 20 5 -7 1 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4871.75 249.017 18 -8 -3 4 5976.57 325.761 31 -8 -3 4 5273.77 253.558 29 8 3 -4 5333.85 271.971 28 -8 -3 4 5322.29 321.741 14 8 3 -3 2862.11 225.579 32 -8 -3 3 2764.90 220.546 31 -8 -3 3 2871.84 175.997 29 8 3 -3 2761.82 212.813 28 -8 -3 3 3103.39 248.409 14 -8 -3 3 2453.88 181.272 11 8 3 -2 7110.64 345.060 32 -8 -3 2 7017.05 327.779 31 8 3 -2 6925.22 324.452 28 -8 -3 2 7174.83 339.743 14 -8 -3 2 6685.57 270.772 11 8 3 -1 38649.5 734.805 32 8 3 -1 39371.5 744.555 28 -8 -3 1 39532.0 700.387 14 -8 -3 1 37859.5 582.805 11 8 3 0 74.5942 43.4388 32 8 3 0 69.0732 47.3031 28 -8 -3 0 116.113 45.6197 14 8 4 -6 11982.7 308.899 32 -8 -4 6 12952.8 337.109 31 8 4 -5 2124.37 145.398 32 -8 -4 5 2216.01 153.986 31 -8 -4 5 1875.64 134.676 14 8 4 -4 10012.4 325.397 32 -8 -4 4 9697.76 324.033 31 8 4 -4 9043.54 262.374 28 -8 -4 4 9386.92 311.078 14 8 4 -3 10631.0 336.364 32 -8 -4 3 10763.8 333.002 31 8 4 -3 10242.0 297.737 28 -8 -4 3 10466.5 327.239 14 8 4 -2 83.7864 39.4626 32 8 4 -2 17.7319 37.7707 28 -8 -4 2-23.3370 38.8894 14 8 4 -1 5540.99 205.585 28 9 -8 -5 67.5319 41.3997 18 9 -8 -5 41.7569 36.5449 28 -9 8 5 67.6334 41.9683 26 9 -8 -4 13306.4 353.130 18 -9 8 4 13326.2 308.009 30 -9 8 4 13359.5 357.639 26 9 -8 -3 6982.43 264.176 18 -9 8 3 6670.98 217.638 30 -9 8 3 7164.17 260.052 26 9 -8 -2 167.769 49.8752 18 -9 8 2 115.344 46.6703 26 9 -8 -1 13940.3 316.038 18 9 -8 -1 14037.9 301.851 27 -9 8 1 14794.4 335.112 13 9 -7 -7 19417.5 346.440 15 -9 7 7 19815.6 394.209 26 9 -7 -6 3468.70 174.960 18 9 -7 -6 3774.40 211.744 28 9 -7 -6 3326.36 151.676 15 -9 7 6 3382.05 187.425 26 9 -7 -5 10073.9 324.078 18 9 -7 -5 10571.8 353.824 28 -9 7 5 10371.8 342.167 26 9 -7 -4 10089.3 337.988 18 9 -7 -4 10285.7 344.544 28 -9 7 4 9840.60 347.054 26 9 -7 -3 6863.33 286.866 18 9 -7 -3 7488.17 280.567 28 -9 7 3 7451.03 299.591 26 9 -7 -2 19059.5 471.515 18 9 -7 -2 20410.6 429.898 28 9 -7 -2 19346.0 415.819 27 -9 7 2 19086.9 458.502 26 9 -7 -1 818.948 108.754 18 9 -7 -1 936.488 103.005 27 -9 7 1 951.017 96.0638 26 -9 7 1 597.114 106.114 13 9 -7 0 31587.4 519.704 27 -9 7 0 31770.7 531.437 13 9 -7 1 19841.2 377.115 27 -9 7 -1 20298.8 376.386 13 9 -6 -8 230.677 64.5065 28 9 -6 -8 187.904 55.6008 15 9 -6 -7 291.883 60.1652 18 9 -6 -7 167.802 69.1324 28 -9 6 7 343.760 81.6027 26 9 -6 -6 3849.53 200.659 18 9 -6 -6 4576.44 232.322 28 -9 6 6 4048.38 222.846 26 9 -6 -5 6260.19 269.858 18 9 -6 -5 6117.41 269.124 28 -9 6 5 6004.67 283.459 26 9 -6 -4 4912.02 247.082 18 9 -6 -4 4857.31 239.227 28 -9 6 4 4885.85 260.058 26 9 -6 -3 14254.7 420.424 18 9 -6 -3 14325.4 397.247 28 9 -6 -3 14057.3 367.059 27 -9 6 3 13889.2 428.956 26 9 -6 -2 7657.39 306.754 18 9 -6 -2 8406.22 284.018 28 9 -6 -2 8730.27 306.320 27 -9 6 2 7983.53 312.647 26 -9 6 2 7612.46 273.177 12 9 -6 -1 9846.11 333.594 18 9 -6 -1 10039.4 328.509 27 -9 6 1 9623.20 308.954 26 -9 6 1 9146.11 360.250 13 -9 6 1 9585.08 312.420 12 9 -6 0 7.08821 50.6782 18 9 -6 0 192.953 79.8893 27 -9 6 0 101.440 59.0712 13 -9 6 0 118.333 57.1734 12 9 -6 1 22015.8 440.364 27 -9 6 -1 21793.6 444.226 13 -9 6 -1 20752.1 438.789 12 9 -6 2 6411.94 207.992 27 -9 6 -2 7122.94 220.854 13 9 -5 -8 10459.6 300.799 32 -9 5 8 9998.65 316.610 26 9 -5 -7 10322.7 312.373 32 9 -5 -7 10741.8 320.273 18 9 -5 -7 10777.0 348.747 28 -9 5 7 10505.1 361.115 26 9 -5 -6 577.921 82.2339 32 9 -5 -6 597.510 91.0855 18 9 -5 -6 615.870 98.4586 28 -9 5 6 765.677 125.241 26 9 -5 -5 607.612 107.004 18 9 -5 -5 786.144 110.249 28 -9 5 5 575.980 114.830 26 9 -5 -4 44266.7 759.581 18 9 -5 -4 43061.4 739.826 28 -9 5 4 42018.1 782.991 26 9 -5 -3 10584.3 368.622 18 -9 5 3 11018.1 350.259 29 9 -5 -3 10229.2 354.863 28 9 -5 -3 10774.4 341.651 27 -9 5 3 9967.02 373.706 26 9 -5 -2 14716.0 422.859 18 -9 5 2 15449.3 422.929 29 9 -5 -2 15427.5 411.094 28 9 -5 -2 15741.5 435.184 27 -9 5 2 14727.9 427.052 26 9 -5 -1 19327.0 462.276 18 9 -5 -1 21101.9 431.607 28 9 -5 -1 20058.6 494.088 27 -9 5 1 19950.3 537.775 13 9 -5 0 8574.69 287.854 18 9 -5 0 9278.03 322.488 27 -9 5 0 9363.28 330.355 13 -9 5 0 8793.96 318.251 12 9 -5 1 5878.33 239.911 27 -9 5 -1 5642.87 239.267 13 -9 5 -1 5478.28 240.917 12 -9 5 -2 11497.2 300.374 13 -9 5 -2 10890.1 315.628 12 9 -4 -9 9280.07 279.482 32 -9 4 9 8632.25 272.010 26 9 -4 -8 10145.6 321.798 32 9 -4 -8 10012.7 295.932 18 9 -4 -8 11265.0 300.921 10 9 -4 -8 11076.0 325.904 28 -9 4 8 10500.5 353.890 26 9 -4 -7 11760.1 364.576 32 9 -4 -7 12945.8 380.425 18 9 -4 -7 12498.0 358.629 10 9 -4 -7 12670.8 378.885 28 -9 4 7 13153.6 423.172 26 9 -4 -6 8331.66 311.155 32 9 -4 -6 9138.38 344.552 18 9 -4 -6 9066.07 343.099 28 -9 4 6 8492.27 368.028 26 9 -4 -5 3784.51 202.925 32 9 -4 -5 4084.83 242.799 18 -9 4 5 4090.59 224.912 29 9 -4 -5 3871.18 231.994 28 9 -4 -4 6010.28 296.400 18 -9 4 4 6404.64 291.471 29 9 -4 -4 6072.57 291.892 28 -9 4 4 5875.37 296.534 26 9 -4 -3 38718.7 716.294 18 9 -4 -3 37392.9 704.674 28 9 -4 -3 37372.0 662.959 27 -9 4 3 36501.0 707.401 26 -9 4 3 38563.5 693.684 11 9 -4 -2 1939.84 160.542 18 -9 4 2 1868.02 169.383 29 9 -4 -2 1724.19 150.134 28 9 -4 -2 1441.55 163.928 27 -9 4 2 1694.64 144.661 26 -9 4 2 1162.25 147.416 13 -9 4 2 2192.89 165.722 11 9 -4 -1 16828.6 421.853 18 -9 4 1 17262.8 492.023 29 9 -4 -1 17647.3 423.653 28 9 -4 -1 17881.7 462.474 27 -9 4 1 17897.9 468.663 13 -9 4 1 17686.4 429.184 11 -9 4 0 18404.5 484.637 29 9 -4 0 19602.7 468.832 27 -9 4 0 18750.0 458.666 13 -9 4 0 18541.9 411.884 11 9 -4 1 8869.20 298.456 27 -9 4 -1 8574.73 289.583 13 -9 4 -1 8314.02 303.453 12 -9 4 -2 6768.35 230.737 13 -9 4 -2 6544.85 247.651 12 9 -3 -9 17889.1 401.625 32 9 -3 -9 19016.6 379.758 10 -9 3 9 17743.8 418.195 26 9 -3 -8 2121.55 159.365 32 9 -3 -8 2254.70 151.605 18 9 -3 -8 2171.57 142.603 28 -9 3 8 2071.82 167.600 26 9 -3 -7 13347.5 406.814 32 9 -3 -7 13511.6 406.197 18 -9 3 7 13753.3 384.908 29 9 -3 -7 13546.1 393.552 28 -9 3 7 13080.4 443.739 26 9 -3 -6 17832.8 481.111 32 9 -3 -6 19701.3 518.829 18 -9 3 6 19440.4 508.359 29 9 -3 -6 19054.6 501.270 28 -9 3 6 18603.8 542.187 26 9 -3 -5 10304.2 362.216 32 9 -3 -5 10764.4 398.025 18 -9 3 5 10717.5 406.951 29 9 -3 -5 10951.2 394.220 28 -9 3 5 10597.5 411.062 26 9 -3 -4 1418.78 132.427 32 9 -3 -4 1291.64 144.620 18 -9 3 4 1565.94 163.316 29 9 -3 -4 1566.83 162.198 28 -9 3 4 1413.89 155.763 26 9 -3 -3 31006.4 644.849 18 -9 3 3 31488.8 711.027 29 9 -3 -3 31106.8 661.841 28 -9 3 3 30763.0 626.088 26 -9 3 3 30289.3 695.898 11 9 -3 -2 15333.1 428.388 18 -9 3 2 15745.0 500.759 29 9 -3 -2 15967.0 458.694 28 -9 3 2 16406.3 415.777 13 -9 3 2 15489.3 476.153 11 9 -3 -1 2629.02 161.608 18 -9 3 1 2735.37 205.328 29 9 -3 -1 2628.84 174.473 28 -9 3 1 2880.30 174.223 13 -9 3 1 2747.00 196.232 11 -9 3 0 13324.7 429.873 29 9 -3 0 13571.2 335.190 28 9 -3 0 14144.4 418.224 27 -9 3 0 13424.2 356.701 13 -9 3 0 13270.7 387.468 11 9 -3 1 18029.2 429.022 27 -9 3 -1 18421.7 394.024 13 -9 3 -1 17016.7 426.919 12 -9 3 -1 18182.7 413.399 11 9 -3 2 965.799 88.9491 27 -9 3 -2 1617.74 123.457 12 9 -2 -9 4906.24 210.155 32 9 -2 -9 4433.40 177.584 18 9 -2 -9 4897.51 211.019 10 -9 2 9 5228.05 235.883 26 9 -2 -8 24953.8 536.642 32 9 -2 -8 25348.1 516.697 18 -9 2 8 25874.2 521.958 29 9 -2 -8 25260.4 448.213 28 -9 2 8 26296.8 588.214 26 9 -2 -7 1764.93 159.851 32 9 -2 -7 1746.42 159.301 18 -9 2 7 1442.25 147.620 29 9 -2 -7 1682.68 138.974 28 -9 2 7 1701.05 165.987 26 9 -2 -6 2333.87 186.009 32 9 -2 -6 2362.33 199.196 18 -9 2 6 2420.70 200.779 29 9 -2 -6 2365.73 182.169 28 -9 2 6 2441.77 195.581 26 9 -2 -5 17766.4 495.411 32 9 -2 -5 18365.1 518.380 18 -9 2 5 18685.7 556.959 29 9 -2 -5 18848.4 525.415 28 -9 2 5 17149.9 511.142 26 9 -2 -4 6311.34 286.807 32 9 -2 -4 6571.14 305.629 18 -9 2 4 6177.07 327.858 29 9 -2 -4 6480.00 311.936 28 -9 2 4 5702.90 282.869 26 9 -2 -3 370.950 73.1553 32 9 -2 -3 299.398 82.8074 18 -9 2 3 370.183 108.241 29 9 -2 -3 269.593 86.7672 28 -9 2 3 243.438 122.557 11 9 -2 -2 23385.9 507.980 18 -9 2 2 23893.9 614.649 29 9 -2 -2 24961.4 581.068 28 -9 2 2 22859.9 620.298 11 -9 2 1 20072.5 543.749 29 9 -2 -1 19726.7 478.259 28 -9 2 1 19668.8 533.079 11 -9 2 0 914.947 123.055 29 9 -2 0 1145.09 106.019 28 -9 2 0 954.227 113.553 11 -9 2 -1 7156.25 270.135 12 -9 2 -1 8491.94 295.484 11 9 -2 2 6478.84 227.244 27 -9 2 -2 10314.2 293.754 11 9 -1 -9 6789.58 235.698 32 -9 1 9 6452.57 259.252 26 9 -1 -8 3696.87 205.508 32 9 -1 -8 3776.93 207.663 18 -9 1 8 4136.19 241.409 29 -9 1 8 4061.58 251.220 26 9 -1 -7 30399.4 627.536 32 9 -1 -7 31375.6 636.502 18 -9 1 7 31918.3 728.203 29 9 -1 -7 29483.6 535.156 28 -9 1 7 31129.6 686.969 26 9 -1 -6-41.2823 82.5346 32 9 -1 -6 102.226 85.9984 18 -9 1 6 5.29208 84.4883 29 9 -1 -6-2.94360 68.6073 28 -9 1 6 87.6429 80.9486 26 9 -1 -5 29095.8 647.475 32 9 -1 -5 27790.5 630.976 18 -9 1 5 27440.0 694.449 29 9 -1 -5 28411.6 638.594 28 9 -1 -4 11731.9 404.769 32 9 -1 -4 12541.4 413.216 18 -9 1 4 12427.2 463.917 29 9 -1 -4 12816.3 437.117 28 -9 1 4 12286.2 412.083 14 9 -1 -3 3623.87 211.531 32 9 -1 -3 3783.21 218.057 18 -9 1 3 3701.91 254.823 29 9 -1 -3 3951.46 246.271 28 -9 1 3 3697.76 235.552 14 -9 1 3 2858.58 262.896 11 9 -1 -2 9806.25 304.743 18 -9 1 2 10236.3 396.409 29 9 -1 -2 9895.45 365.820 28 -9 1 2 9843.25 402.750 11 -9 1 1 19806.5 520.554 29 9 -1 -1 19282.8 472.204 28 -9 1 1 19877.4 530.592 11 -9 1 0 20226.1 490.265 29 9 -1 0 20558.9 420.267 28 -9 1 0 20314.5 491.871 11 -9 1 -1 49.5811 40.3603 12 -9 1 -1 110.694 50.6214 11 9 0 -8 155.088 49.5832 32 9 0 -8 192.026 63.2985 18 -9 0 8 110.892 65.0373 29 -9 0 8 302.034 78.0505 26 9 0 -7 6360.13 277.298 32 9 0 -7 6370.15 297.663 18 -9 0 7 6607.09 334.092 29 9 0 -7 6196.67 216.305 28 -9 0 7 6609.54 307.089 26 9 0 -6 15705.0 467.041 32 9 0 -6 15899.2 485.247 18 -9 0 6 17025.6 530.871 29 9 0 -6 15724.2 411.752 28 -9 0 6 15735.5 438.707 26 9 0 -5 339.955 97.6446 32 9 0 -5 382.351 90.1584 18 -9 0 5 410.072 126.397 29 9 0 -5 379.376 87.0285 28 -9 0 5 540.532 95.2978 14 9 0 -4 33100.2 639.867 18 -9 0 4 32913.8 720.823 29 9 0 -4 34239.4 705.334 28 -9 0 4 34541.0 687.889 14 9 0 -3 15676.1 444.857 32 9 0 -3 15492.7 394.064 18 -9 0 3 16667.4 489.309 29 9 0 -3 16017.8 484.333 28 -9 0 3 16939.8 483.478 14 -9 0 3 16156.6 518.165 11 9 0 -2 149.303 48.4130 32 -9 0 2 99.4655 73.1551 29 9 0 -2 120.086 71.9143 28 -9 0 2 38.6614 64.2701 14 -9 0 2 32.2328 80.7541 11 -9 0 1 6123.49 261.831 29 9 0 -1 5485.23 245.401 28 -9 0 1 6169.76 274.944 11 -9 0 0 16610.2 381.936 29 -9 0 0 16575.5 406.932 11 -9 0 -1 7032.42 233.727 11 9 1 -7 7261.88 257.839 32 9 1 -7 6765.74 264.648 18 -9 -1 7 7241.98 272.378 29 9 1 -6 4338.65 225.541 32 9 1 -6 4436.27 239.691 18 -9 -1 6 4176.60 230.103 29 9 1 -6 4185.60 178.998 28 9 1 -5 20307.2 514.514 32 9 1 -5 21909.4 493.354 18 -9 -1 5 21660.6 507.399 29 9 1 -5 20938.7 451.454 28 9 1 -4 11611.8 410.260 32 9 1 -4 11369.5 318.547 18 -9 -1 4 12122.1 376.006 29 9 1 -4 12121.6 377.692 28 -9 -1 4 12239.3 438.693 14 -9 -1 4 11265.6 394.896 11 9 1 -3 8229.86 350.574 32 -9 -1 3 9587.36 322.582 29 9 1 -3 10835.0 389.053 28 -9 -1 3 9664.56 374.237 14 -9 -1 3 9390.80 338.305 11 -9 -1 2 12161.8 336.190 29 9 1 -2 12947.0 432.874 28 -9 -1 2 12198.2 374.805 14 -9 -1 2 12546.5 362.593 11 9 1 -1 87.6958 47.7692 28 -9 -1 1-24.3833 42.5862 11 9 2 -5 13837.2 340.736 32 9 2 -4 6091.26 230.185 32 9 2 -4 5771.60 206.395 28 -9 -2 4 6044.78 221.421 14 9 2 -3 7971.85 245.324 28 -9 -2 3 7638.70 250.255 14 10 -4 -5 1793.05 113.166 18 10 -4 -5 1660.94 108.865 28 10 -4 -4 2100.31 120.659 18 10 -4 -4 2198.90 121.762 28 10 -3 -5 3647.36 158.402 18 10 -3 -5 3622.99 162.196 28 10 -3 -4 90.5260 35.9618 28 0 0 0 0.00 0.00 0 TITL REARDG in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 8.067362 10.041331 11.450902 90.2651 105.7869 106.8797 ZERR 2.00 0.000340 0.000473 0.000468 0.0036 0.0038 0.0040 LATT 1 SFAC C H O Br UNIT 38.00 38.00 6.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 8778 _olex2_date_sample_data_collection 2018-02-20 _olex2_date_sample_submission 2018-01-16 _olex2_submission_original_sample_id RA-320-001 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.253 _oxdiff_exptl_absorpt_empirical_full_min 0.710 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.64606(14) 0.71997(12) 0.32510(11) 0.0198(2) Uani 1 1 d . . . . . C2 C 0.7119(2) 0.61153(16) 0.38244(15) 0.0197(3) Uani 1 1 d . . . . . H2 H 0.622112 0.555360 0.422530 0.024 Uiso 1 1 calc R . . . . C3 C 0.8897(2) 0.67307(16) 0.47845(15) 0.0189(3) Uani 1 1 d . . . . . H3A H 0.931040 0.596371 0.518083 0.023 Uiso 1 1 calc R . . . . H3B H 0.872002 0.730773 0.541622 0.023 Uiso 1 1 calc R . . . . C4 C 1.0385(2) 0.76477(16) 0.42527(14) 0.0165(3) Uani 1 1 d . . . . . C5 C 0.9543(2) 0.85029(16) 0.32955(14) 0.0168(3) Uani 1 1 d . . . . . C6 C 1.0657(2) 0.95881(17) 0.28476(15) 0.0197(3) Uani 1 1 d . . . . . H6 H 1.192995 0.978380 0.315012 0.024 Uiso 1 1 calc R . . . . C7 C 0.9964(2) 1.03933(17) 0.19724(15) 0.0208(3) Uani 1 1 d . . . . . C8 C 0.8092(2) 1.01193(17) 0.15601(15) 0.0208(3) Uani 1 1 d . . . . . H8 H 0.758331 1.066725 0.097681 0.025 Uiso 1 1 calc R . . . . C9 C 0.6978(2) 0.90465(17) 0.20041(14) 0.0186(3) Uani 1 1 d . . . . . C10 C 0.7670(2) 0.82186(16) 0.28591(14) 0.0168(3) Uani 1 1 d . . . . . O11 O 0.73141(15) 0.52315(12) 0.29600(11) 0.0221(2) Uani 1 1 d . . . . . C12 C 0.5641(2) 0.45698(19) 0.20373(17) 0.0276(4) Uani 1 1 d . . . . . H12A H 0.525105 0.527406 0.152114 0.033 Uiso 1 1 calc R . . . . H12B H 0.468336 0.411958 0.242267 0.033 Uiso 1 1 calc R . . . . C13 C 0.5946(3) 0.3497(2) 0.1277(2) 0.0391(5) Uani 1 1 d . . . . . H13A H 0.482816 0.304494 0.063292 0.059 Uiso 1 1 calc GR . . . . H13B H 0.630358 0.279257 0.179192 0.059 Uiso 1 1 calc GR . . . . H13C H 0.690641 0.394994 0.090840 0.059 Uiso 1 1 calc GR . . . . C14 C 1.1785(2) 0.86060(17) 0.52979(15) 0.0202(3) Uani 1 1 d . . . . . H14 H 1.145207 0.930105 0.566371 0.024 Uiso 1 1 calc R . . . . C15 C 1.3464(2) 0.85430(18) 0.57440(15) 0.0228(3) Uani 1 1 d . . . . . H15 H 1.427142 0.918324 0.641106 0.027 Uiso 1 1 calc R . . . . C16 C 1.4099(2) 0.75070(18) 0.52293(15) 0.0221(3) Uani 1 1 d . . . . . C17 C 1.2860(2) 0.66766(17) 0.41058(15) 0.0208(3) Uani 1 1 d . . . . . H17 H 1.326847 0.607698 0.368502 0.025 Uiso 1 1 calc R . . . . C18 C 1.1181(2) 0.67385(16) 0.36589(14) 0.0177(3) Uani 1 1 d . . . . . H18 H 1.044315 0.618023 0.292629 0.021 Uiso 1 1 calc R . . . . O19 O 1.55674(17) 0.73393(16) 0.57195(12) 0.0319(3) Uani 1 1 d . . . . . C20 C 1.1241(2) 1.15015(19) 0.14643(17) 0.0271(4) Uani 1 1 d . . . . . H20A H 1.239208 1.189244 0.211469 0.033 Uiso 1 1 calc R . . . . H20B H 1.151055 1.104854 0.079828 0.033 Uiso 1 1 calc R . . . . C21 C 1.0547(3) 1.26745(19) 0.09871(18) 0.0305(4) Uani 1 1 d . . . . . H21 H 1.020261 1.318853 0.152868 0.037 Uiso 1 1 calc R . . . . C22 C 1.0376(3) 1.3051(2) -0.0126(2) 0.0384(5) Uani 1 1 d . . . . . H22A H 1.070700 1.256232 -0.069412 0.046 Uiso 1 1 calc R . . . . H22B H 0.992216 1.381228 -0.036317 0.046 Uiso 1 1 calc R . . . . Br23 Br 0.44335(2) 0.86941(2) 0.14596(2) 0.02289(7) 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 O1 0.0137(5) 0.0217(5) 0.0246(6) 0.0050(5) 0.0067(4) 0.0050(4) C2 0.0169(7) 0.0211(7) 0.0231(8) 0.0036(6) 0.0086(6) 0.0063(6) C3 0.0179(7) 0.0223(7) 0.0194(8) 0.0034(6) 0.0082(6) 0.0076(6) C4 0.0136(7) 0.0181(7) 0.0174(7) 0.0001(6) 0.0039(6) 0.0049(6) C5 0.0155(7) 0.0190(7) 0.0156(7) -0.0008(6) 0.0037(6) 0.0056(6) C6 0.0139(7) 0.0237(8) 0.0189(8) 0.0003(6) 0.0028(6) 0.0037(6) C7 0.0192(8) 0.0212(7) 0.0193(8) 0.0005(6) 0.0044(6) 0.0029(6) C8 0.0214(8) 0.0226(8) 0.0165(8) 0.0014(6) 0.0019(6) 0.0071(6) C9 0.0139(7) 0.0229(7) 0.0172(7) -0.0013(6) 0.0015(6) 0.0059(6) C10 0.0151(7) 0.0179(7) 0.0168(7) -0.0015(6) 0.0048(6) 0.0040(6) O11 0.0165(5) 0.0226(5) 0.0261(6) -0.0023(5) 0.0070(5) 0.0035(4) C12 0.0201(8) 0.0305(9) 0.0270(9) -0.0034(7) 0.0045(7) 0.0019(7) C13 0.0350(11) 0.0409(11) 0.0360(11) -0.0124(9) 0.0105(9) 0.0032(9) C14 0.0207(8) 0.0213(7) 0.0186(8) 0.0011(6) 0.0049(6) 0.0070(6) C15 0.0190(8) 0.0265(8) 0.0183(8) -0.0025(6) 0.0006(6) 0.0042(6) C16 0.0160(7) 0.0316(9) 0.0196(8) 0.0041(7) 0.0059(6) 0.0074(6) C17 0.0182(8) 0.0256(8) 0.0218(8) 0.0025(6) 0.0089(6) 0.0084(6) C18 0.0165(7) 0.0198(7) 0.0176(7) 0.0013(6) 0.0064(6) 0.0050(6) O19 0.0190(6) 0.0540(8) 0.0246(6) 0.0005(6) 0.0030(5) 0.0171(6) C20 0.0208(8) 0.0300(9) 0.0255(9) 0.0071(7) 0.0046(7) 0.0019(7) C21 0.0305(9) 0.0246(8) 0.0339(10) 0.0041(7) 0.0104(8) 0.0034(7) C22 0.0446(12) 0.0312(10) 0.0347(11) 0.0101(8) 0.0059(9) 0.0096(9) Br23 0.01430(10) 0.03118(11) 0.02145(10) 0.00149(7) 0.00105(7) 0.00808(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0010 0 -1 0 0.0270 0 -1 1 0.0151 0 1 -1 0.0140 4 -2 -5 0.1443 -5 1 1 0.1969 0 -2 -6 0.0396 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 C10 O1 C2 115.91(11) . . ? O1 C2 H2 108.5 . . ? O1 C2 C3 110.57(13) . . ? C3 C2 H2 108.5 . . ? O11 C2 O1 110.47(13) . . ? O11 C2 H2 108.5 . . ? O11 C2 C3 110.11(13) . . ? C2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C2 C3 C4 112.53(13) . . ? H3A C3 H3B 107.8 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C5 C4 C3 109.07(12) . . ? C14 C4 C3 106.66(13) . . ? C14 C4 C5 110.01(12) . . ? C14 C4 C18 111.68(13) . . ? C18 C4 C3 110.41(12) . . ? C18 C4 C5 108.97(12) . . ? C6 C5 C4 119.74(13) . . ? C6 C5 C10 119.08(14) . . ? C10 C5 C4 121.18(13) . . ? C5 C6 H6 118.9 . . ? C7 C6 C5 122.16(15) . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 118.32(14) . . ? C6 C7 C20 119.67(15) . . ? C8 C7 C20 121.98(15) . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.79(15) . . ? C9 C8 H8 120.1 . . ? C8 C9 C10 121.88(14) . . ? C8 C9 Br23 119.70(12) . . ? C10 C9 Br23 118.42(12) . . ? O1 C10 C5 123.86(14) . . ? O1 C10 C9 117.35(13) . . ? C9 C10 C5 118.74(14) . . ? C2 O11 C12 112.81(12) . . ? O11 C12 H12A 110.1 . . ? O11 C12 H12B 110.1 . . ? O11 C12 C13 108.13(15) . . ? H12A C12 H12B 108.4 . . ? C13 C12 H12A 110.1 . . ? C13 C12 H12B 110.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C14 H14 117.9 . . ? C15 C14 C4 124.16(15) . . ? C15 C14 H14 117.9 . . ? C14 C15 H15 119.2 . . ? C14 C15 C16 121.59(16) . . ? C16 C15 H15 119.2 . . ? C17 C16 C15 116.02(14) . . ? O19 C16 C15 121.75(16) . . ? O19 C16 C17 122.22(16) . . ? C16 C17 H17 119.0 . . ? C18 C17 C16 121.99(15) . . ? C18 C17 H17 119.0 . . ? C4 C18 H18 118.2 . . ? C17 C18 C4 123.60(15) . . ? C17 C18 H18 118.2 . . ? C7 C20 H20A 108.6 . . ? C7 C20 H20B 108.6 . . ? H20A C20 H20B 107.5 . . ? C21 C20 C7 114.84(15) . . ? C21 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C20 C21 H21 117.5 . . ? C22 C21 C20 124.9(2) . . ? C22 C21 H21 117.5 . . ? C21 C22 H22A 120.0 . . ? C21 C22 H22B 120.0 . . ? H22A C22 H22B 120.0 . . ? 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 O1 C2 1.4324(19) . ? O1 C10 1.3649(18) . ? C2 H2 1.0000 . ? C2 C3 1.506(2) . ? C2 O11 1.396(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.555(2) . ? C4 C5 1.531(2) . ? C4 C14 1.502(2) . ? C4 C18 1.510(2) . ? C5 C6 1.395(2) . ? C5 C10 1.397(2) . ? C6 H6 0.9500 . ? C6 C7 1.391(2) . ? C7 C8 1.396(2) . ? C7 C20 1.518(2) . ? C8 H8 0.9500 . ? C8 C9 1.385(2) . ? C9 C10 1.393(2) . ? C9 Br23 1.8997(15) . ? O11 C12 1.441(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.497(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14 0.9500 . ? C14 C15 1.332(2) . ? C15 H15 0.9500 . ? C15 C16 1.469(2) . ? C16 C17 1.468(2) . ? C16 O19 1.226(2) . ? C17 H17 0.9500 . ? C17 C18 1.331(2) . ? C18 H18 0.9500 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.491(3) . ? C21 H21 0.9500 . ? C21 C22 1.314(3) . ? C22 H22A 0.9500 . ? C22 H22B 0.9500 . ? 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 C2 C3 C4 -60.13(16) . . . . ? O1 C2 O11 C12 -59.64(16) . . . . ? C2 O1 C10 C5 -20.4(2) . . . . ? C2 O1 C10 C9 161.84(14) . . . . ? C2 C3 C4 C5 39.92(17) . . . . ? C2 C3 C4 C14 158.70(13) . . . . ? C2 C3 C4 C18 -79.78(16) . . . . ? C2 O11 C12 C13 -171.69(15) . . . . ? C3 C2 O11 C12 177.96(13) . . . . ? C3 C4 C5 C6 168.40(14) . . . . ? C3 C4 C5 C10 -11.53(19) . . . . ? C3 C4 C14 C15 112.85(17) . . . . ? C3 C4 C18 C17 -110.69(17) . . . . ? C4 C5 C6 C7 179.62(14) . . . . ? C4 C5 C10 O1 1.2(2) . . . . ? C4 C5 C10 C9 178.86(14) . . . . ? C4 C14 C15 C16 0.4(3) . . . . ? C5 C4 C14 C15 -128.99(16) . . . . ? C5 C4 C18 C17 129.54(16) . . . . ? C5 C6 C7 C8 1.7(2) . . . . ? C5 C6 C7 C20 -176.27(15) . . . . ? C6 C5 C10 O1 -178.76(14) . . . . ? C6 C5 C10 C9 -1.1(2) . . . . ? C6 C7 C8 C9 -1.5(2) . . . . ? C6 C7 C20 C21 -154.50(16) . . . . ? C7 C8 C9 C10 0.0(2) . . . . ? C7 C8 C9 Br23 179.07(12) . . . . ? C7 C20 C21 C22 -123.3(2) . . . . ? C8 C7 C20 C21 27.6(2) . . . . ? C8 C9 C10 O1 179.17(14) . . . . ? C8 C9 C10 C5 1.3(2) . . . . ? C10 O1 C2 C3 49.16(17) . . . . ? C10 O1 C2 O11 -72.98(16) . . . . ? C10 C5 C6 C7 -0.4(2) . . . . ? O11 C2 C3 C4 62.22(16) . . . . ? C14 C4 C5 C6 51.74(18) . . . . ? C14 C4 C5 C10 -128.19(15) . . . . ? C14 C4 C18 C17 7.8(2) . . . . ? C14 C15 C16 C17 7.6(2) . . . . ? C14 C15 C16 O19 -171.58(17) . . . . ? C15 C16 C17 C18 -7.7(2) . . . . ? C16 C17 C18 C4 -0.3(2) . . . . ? C18 C4 C5 C6 -71.01(18) . . . . ? C18 C4 C5 C10 109.06(16) . . . . ? C18 C4 C14 C15 -7.9(2) . . . . ? O19 C16 C17 C18 171.54(16) . . . . ? C20 C7 C8 C9 176.48(16) . . . . ? Br23 C9 C10 O1 0.04(19) . . . . ? Br23 C9 C10 C5 -177.80(11) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0004 1.0000 0.0007 0.1015 -0.1029 -0.0708 0.0004 -1.0000 -0.0007 -0.1015 0.1029 0.0708 0.0000 -0.9999 0.9969 -0.1519 0.1222 -0.0584 -0.0000 0.9999 -0.9969 0.1519 -0.1222 0.0584 3.9997 -1.9949 -4.9956 0.6173 0.5575 0.3767 -4.9973 0.9931 1.0062 -0.6594 -0.6437 0.3139 0.0028 -2.0007 -5.9868 0.0992 0.0902 0.9170