#------------------------------------------------------------------------------ #$Date: 2021-11-09 00:55:12 +0200 (Tue, 09 Nov 2021) $ #$Revision: 270527 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/92/7129208.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_7129208 loop_ _publ_author_name 'Song, Xianheng' 'Meng, Shanshui' 'Zhang, Hong' 'Jiang, Yi' 'Chan, Albert S. C.' 'Zou, Yong' _publ_section_title ; Dibrominated Addition and Substitution of Alkenes Catalyzed by Mn2(CO)10 ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/D1CC04534B _journal_year 2021 _chemical_formula_moiety 'C16 H14 Br2 O2' _chemical_formula_sum 'C16 H14 Br2 O2' _chemical_formula_weight 398.09 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-03-01 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-05-10 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.6370(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.96300(10) _cell_length_b 6.03520(10) _cell_length_c 16.0210(2) _cell_measurement_reflns_used 11898 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 75.9870 _cell_measurement_theta_min 2.7460 _cell_volume 768.391(19) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.968 _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 113.00 139.00 0.50 0.20 -- 105.44 30.00-101.00 52 2 \w 48.00 97.00 0.50 0.05 -- 46.62 30.00-101.00 98 3 \w 4.00 29.00 0.50 0.05 -- 46.62 -30.00 98.00 50 4 \w 33.00 70.00 0.50 0.20 -- 105.44-125.00 30.00 74 5 \w 77.00 107.00 0.50 0.20 -- 105.44-125.00 30.00 60 6 \w 79.00 105.00 0.50 0.20 -- 105.44 -94.00-150.00 52 7 \w 44.00 70.00 0.50 0.20 -- 105.44 -94.00-150.00 52 8 \w 33.00 69.00 0.50 0.20 -- 105.44 -61.00 60.00 72 9 \w 35.00 72.00 0.50 0.20 -- 105.44 -61.00 120.00 74 10 \w 35.00 68.00 0.50 0.20 -- 105.44 -61.00 90.00 66 11 \w 36.00 65.00 0.50 0.20 -- 105.44 -61.00 150.00 58 12 \w 36.00 62.00 0.50 0.20 -- 105.44 -61.00 30.00 52 13 \w 35.00 63.00 0.50 0.20 -- 105.44 -61.00-150.00 56 14 \w 34.00 70.00 0.50 0.20 -- 105.44 -61.00-180.00 72 15 \w -40.00 20.00 0.50 0.05 -- -46.62 38.00 30.00 120 16 \w -23.00 29.00 0.50 0.05 -- -46.62 19.00 -30.00 104 17 \w -33.00 27.00 0.50 0.05 -- -46.62 30.00-101.00 120 18 \w -66.00 -30.00 0.50 0.20 -- -100.00 61.00 -30.00 72 19 \w -58.00 -33.00 0.50 0.20 -- -100.00 61.00-120.00 50 20 \w -64.00 -38.00 0.50 0.20 -- -100.00 61.00 0.00 52 21 \w -55.00 -29.00 0.50 0.20 -- -100.00 61.00 30.00 52 22 \w -60.00 -35.00 0.50 0.20 -- -100.00 61.00 60.00 50 23 \w -69.00 -43.00 0.50 0.20 -- -100.00 61.00 90.00 52 24 \w -71.00 -33.00 0.50 0.05 -- -46.62 -30.00 98.00 76 25 \w -175.00 -86.00 0.50 0.20 -- -100.00 -30.00 98.00 178 26 \w 52.00 77.00 0.50 0.05 -- 46.37 30.00-101.00 50 27 \w 23.00 80.00 0.50 0.05 -- 46.37 77.00 -30.00 114 28 \w 56.00 95.00 0.50 0.05 -- 46.37 38.00 -60.00 78 29 \w 31.00 74.00 0.50 0.05 -- 46.37 57.00 60.00 86 30 \w -161.00-135.00 0.50 0.20 -- -100.00 -73.00 7.50 52 31 \w -105.00 -79.00 0.50 0.20 -- -100.00 -77.00 0.00 52 32 \w -105.00 -78.00 0.50 0.20 -- -100.00 -73.00 7.50 54 33 \w -128.00 -79.00 0.50 0.20 -- -100.00 -73.00 -22.52 98 34 \w -167.00 -88.00 0.50 0.20 -- -100.00 -15.00 0.00 158 35 \w -103.00 -77.00 0.50 0.20 -- -100.00 -77.00 -60.00 52 36 \w -111.00 -77.00 0.50 0.20 -- -100.00 -77.00 23.80 68 37 \w -111.00 -85.00 0.50 0.20 -- -100.00 -53.00 52.65 52 38 \w -109.00 -76.00 0.50 0.20 -- -100.00 -77.00 60.00 66 39 \w -111.00 -85.00 0.50 0.20 -- -100.00 -61.00 30.00 52 40 \w -102.00 -76.00 0.50 0.20 -- -100.00 -77.00 30.00 52 41 \w -144.00 -79.00 0.50 0.20 -- -100.00 -71.00 -0.31 130 42 \w -164.00-138.00 0.50 0.20 -- -100.00 -72.00 -12.33 52 43 \w -109.00 -78.00 0.50 0.20 -- -100.00 -72.00 -12.33 62 44 \w -171.00-145.00 0.50 0.20 -- -100.00 -54.00 -54.65 52 45 \w -117.00 -77.00 0.50 0.20 -- -100.00 -75.00 -25.56 80 46 \w -112.00 -77.00 0.50 0.20 -- -100.00 -76.00 16.00 70 47 \w -106.00 -81.00 0.50 0.20 -- -100.00 -67.00 64.68 50 48 \w -122.00 -85.00 0.50 0.20 -- -100.00 -54.00 -54.65 74 49 \w -154.00-128.00 0.50 0.20 -- -100.00 -77.00 60.00 52 50 \w -165.00 -86.00 0.50 0.20 -- -100.00 -58.00 17.24 158 51 \w -136.00 -82.00 0.50 0.20 -- -100.00 -61.00 -60.00 108 52 \w -103.00 -77.00 0.50 0.20 -- -100.00 -77.00 -30.00 52 53 \w -164.00-139.00 0.50 0.20 -- -100.00 -77.00 30.00 50 54 \w 97.00 143.00 0.50 0.20 -- 107.00 30.00-120.00 92 55 \w 66.00 104.00 0.50 0.20 -- 107.00 -77.00 -60.00 76 56 \w 73.00 99.00 0.50 0.20 -- 107.00 -77.00-180.00 52 57 \w 35.00 60.00 0.50 0.20 -- 107.00 -77.00-180.00 50 58 \w 62.00 99.00 0.50 0.20 -- 107.00-125.00 60.00 74 59 \w 82.00 107.00 0.50 0.20 -- 107.00 -77.00 120.00 50 60 \w 39.00 69.00 0.50 0.20 -- 107.00 -77.00 120.00 60 61 \w 36.00 72.00 0.50 0.20 -- 107.00 -61.00-120.00 72 62 \w -118.00 -30.00 0.50 0.05 -- -46.37 -57.00 -60.00 176 63 \w -118.00 -30.00 0.50 0.05 -- -46.37 -57.00 60.00 176 64 \w -118.00 -23.00 0.50 0.05 -- -46.37 -77.00 30.00 190 65 \w -118.00 -30.00 0.50 0.05 -- -46.37 -57.00-120.00 176 66 \w -118.00 -23.00 0.50 0.05 -- -46.37 -77.00-180.00 190 67 \w 18.00 95.00 0.50 0.05 -- 46.37-125.00 60.00 154 68 \w 30.00 74.00 0.50 0.05 -- 46.37 57.00 120.00 88 69 \w 23.00 118.00 0.50 0.05 -- 46.37 77.00-120.00 190 70 \w 18.00 95.00 0.50 0.05 -- 46.37-125.00 120.00 154 71 \w 23.00 118.00 0.50 0.05 -- 46.37 77.00 150.00 190 72 \w -20.00 5.00 0.50 0.05 -- 46.37 -30.00 98.00 50 73 \w -103.00 -77.00 0.50 0.20 -- -100.00 -74.00 -16.96 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0304032000 _diffrn_orient_matrix_UB_12 -0.0982294000 _diffrn_orient_matrix_UB_13 0.0865203000 _diffrn_orient_matrix_UB_21 -0.1912696000 _diffrn_orient_matrix_UB_22 0.0033820000 _diffrn_orient_matrix_UB_23 -0.0218939000 _diffrn_orient_matrix_UB_31 0.0104596000 _diffrn_orient_matrix_UB_32 -0.2355930000 _diffrn_orient_matrix_UB_33 -0.0361734000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 15800 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.939 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.041 _diffrn_reflns_theta_min 2.764 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.678 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.721 _exptl_crystal_description block _exptl_crystal_F_000 392 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.455 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.079 _refine_ls_abs_structure_details ; Flack x determined using 1260 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.04(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 183 _refine_ls_number_reflns 3060 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.112 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0280 _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^)+(0.0184P)^2^+1.1540P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0676 _reflns_Friedel_coverage 0.766 _reflns_Friedel_fraction_full 0.969 _reflns_Friedel_fraction_max 0.903 _reflns_number_gt 2989 _reflns_number_total 3060 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1cc04534b2.cif _cod_data_source_block songxh_210301 _cod_database_code 7129208 _shelx_shelxl_version_number 2018/3 _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 0.731 _shelx_estimated_absorpt_t_min 0.555 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C17(H17), C18(H18), C2(H2), C15(H15), C5(H5), C3(H3), C14(H14), C6(H6) 2.b Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C12(H12A,H12B,H12C) ; _shelx_res_file ; TITL songxh_210301_a.res in P2(1) songxh_210301.res created by SHELXL-2018/3 at 14:53:47 on 01-Mar-2021 REM Old TITL songxh_210301 in P2(1) REM SHELXT solution in P2(1): R1 0.060, Rweak 0.034, Alpha 0.006 REM 0.927 for 4 systematic absences, Orientation as input REM Flack x = -0.033 ( 0.019 ) from 1268 Parsons' quotients REM Formula found by SHELXT: C12 O11 Br9 CELL 1.54184 7.963 6.0352 16.021 90 93.637 90 ZERR 2 0.0001 0.0001 0.0002 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Br O UNIT 32 28 4 4 L.S. 4 PLAN 4 SIZE 0.05 0.05 0.1 CONF MORE -1 BOND $H fmap 2 acta htab REM REM REM WGHT 0.018400 1.154000 FVAR 0.74328 BR10 3 1.072127 0.708318 0.904298 11.00000 0.02684 0.03406 = 0.02337 -0.00149 0.00056 0.00057 BR9 3 1.171970 0.908582 0.730362 11.00000 0.02648 0.03435 = 0.03043 -0.00075 0.00889 -0.00312 O19 4 0.463876 0.091306 0.931529 11.00000 0.02867 0.03110 = 0.03026 0.00493 0.00908 0.00116 O11 4 0.691635 0.705306 0.405399 11.00000 0.04067 0.04580 = 0.02009 0.00135 0.00247 0.01362 C16 1 0.556868 0.230076 0.886336 11.00000 0.03024 0.02794 = 0.01821 0.00024 0.00339 -0.00145 C17 1 0.717176 0.152026 0.868662 11.00000 0.03263 0.02438 = 0.02849 0.00288 0.00409 0.00470 AFIX 43 H17 2 0.752641 0.012214 0.886699 11.00000 -1.20000 AFIX 0 C18 1 0.821727 0.284357 0.824318 11.00000 0.02836 0.02729 = 0.02595 0.00054 0.00784 0.00554 AFIX 43 H18 2 0.927458 0.231814 0.812575 11.00000 -1.20000 AFIX 0 C8 1 1.020090 0.731026 0.786964 11.00000 0.02687 0.02587 = 0.02674 -0.00335 0.00375 0.00081 C2 1 0.888031 0.506245 0.600988 11.00000 0.02868 0.03190 = 0.02356 0.00224 0.00221 0.00695 AFIX 43 H2 2 0.953068 0.385818 0.619499 11.00000 -1.20000 AFIX 0 C7 1 0.885767 0.637184 0.749284 11.00000 0.02499 0.02040 = 0.02274 -0.00091 0.00466 0.00481 C4 1 0.738298 0.704784 0.488664 11.00000 0.02608 0.03532 = 0.02023 0.00286 0.00459 0.00188 C13 1 0.772227 0.494037 0.796943 11.00000 0.02117 0.02964 = 0.01650 -0.00393 -0.00169 0.00042 C1 1 0.841386 0.665934 0.658032 11.00000 0.02295 0.02804 = 0.02246 0.00142 0.00060 -0.00263 C15 1 0.504565 0.438691 0.858105 11.00000 0.02250 0.03186 = 0.02348 -0.00003 0.00366 -0.00035 AFIX 43 H15 2 0.398578 0.491151 0.869433 11.00000 -1.20000 AFIX 0 C5 1 0.692376 0.865033 0.545281 11.00000 0.03526 0.02892 = 0.02454 0.00594 0.00548 0.00837 AFIX 43 H5 2 0.627351 0.985737 0.527051 11.00000 -1.20000 AFIX 0 C3 1 0.838003 0.526003 0.516850 11.00000 0.03601 0.03657 = 0.02029 -0.00231 0.00264 0.01044 AFIX 43 H3 2 0.870890 0.419973 0.479052 11.00000 -1.20000 AFIX 0 C20 1 0.310948 0.179152 0.960397 11.00000 0.02661 0.03750 = 0.02717 0.00336 0.00537 0.00118 AFIX 137 H20A 2 0.230620 0.199091 0.913745 11.00000 -1.50000 H20B 2 0.333306 0.319279 0.987200 11.00000 -1.50000 H20C 2 0.266364 0.077994 0.999604 11.00000 -1.50000 AFIX 0 C14 1 0.610989 0.568328 0.812988 11.00000 0.02474 0.02768 = 0.02089 0.00266 -0.00024 0.00018 AFIX 43 H14 2 0.574598 0.706181 0.793210 11.00000 -1.20000 AFIX 0 C6 1 0.744465 0.843315 0.629341 11.00000 0.04223 0.03140 = 0.02475 -0.00339 0.00716 0.00580 AFIX 43 H6 2 0.713383 0.950553 0.667091 11.00000 -1.20000 AFIX 0 C12 1 0.590849 0.887065 0.373794 11.00000 0.05515 0.06357 = 0.02860 0.00922 0.00390 0.02349 AFIX 137 H12A 2 0.564243 0.866858 0.315003 11.00000 -1.50000 H12B 2 0.652084 1.022912 0.382737 11.00000 -1.50000 H12C 2 0.488683 0.893229 0.402461 11.00000 -1.50000 AFIX 0 HKLF 4 REM songxh_210301_a.res in P2(1) REM wR2 = 0.0676, GooF = S = 1.113, Restrained GooF = 1.112 for all data REM R1 = 0.0280 for 2989 Fo > 4sig(Fo) and 0.0286 for all 3060 data REM 183 parameters refined using 1 restraints END WGHT 0.0184 1.1521 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C17 Br10_$1 EQIV $2 x-1, y, z HTAB C15 Br10_$2 EQIV $3 -x+1, y+1/2, -z+2 HTAB C20 O19_$3 REM Highest difference peak 0.455, deepest hole -0.473, 1-sigma level 0.079 Q1 1 0.7995 0.0006 0.9027 11.00000 0.05 0.46 Q2 1 0.9406 0.7309 0.8602 11.00000 0.05 0.35 Q3 1 1.1895 0.6932 0.9630 11.00000 0.05 0.35 Q4 1 1.0346 0.7118 0.8203 11.00000 0.05 0.35 ; _shelx_res_checksum 10108 _shelx_hkl_file ; 0 -7 0 1.73 3.00 0 -7 0 -0.39 2.55 0 -7 0 0.74 4.57 0 -7 1 32.89 5.63 0 -7 -1 36.12 5.93 0 -7 1 17.15 6.87 0 -7 -1 34.39 5.41 0 -7 -1 36.92 7.60 0 -7 1 27.17 4.94 0 -7 -2 211.41 13.79 0 -7 2 160.72 12.53 0 -7 -2 198.81 13.04 0 -7 2 167.01 16.63 0 -7 2 145.77 11.61 0 -7 -3 331.40 19.40 0 -7 3 296.32 17.95 0 -7 4 2.23 2.37 0 -7 4 -0.73 4.45 0 -7 5 106.71 8.75 0 -7 5 86.86 11.06 0 -7 6 15.05 3.36 0 -7 6 21.41 5.51 0 -7 7 2.66 1.90 0 -7 7 -0.41 2.38 0 -6 0 669.02 37.08 0 -6 0 640.07 44.58 0 -6 0 672.33 36.66 0 -6 -1 30.07 7.18 0 -6 -1 29.89 6.71 0 -6 1 41.24 7.37 0 -6 1 35.14 11.59 0 -6 -1 42.03 11.20 0 -6 -2 237.07 18.54 0 -6 -2 224.78 22.79 0 -6 2 233.66 17.85 0 -6 -2 240.35 18.18 0 -6 -3 8.59 4.73 0 -6 3 1.74 3.82 0 -6 3 3.88 5.95 0 -6 -3 -1.03 5.49 0 -6 3 2.38 3.65 0 -6 3 1.32 8.11 0 -6 4 141.32 13.34 0 -6 -4 164.49 15.02 0 -6 4 175.38 19.00 0 -6 4 186.82 22.03 0 -6 4 188.06 14.82 0 -6 -5 262.03 19.74 0 -6 5 264.44 18.61 0 -6 5 278.69 24.38 0 -6 5 264.68 18.60 0 -6 5 267.69 26.47 0 -6 -6 310.63 21.14 0 -6 6 289.33 19.78 0 -6 6 285.37 25.14 0 -6 6 308.73 19.85 0 -6 6 328.57 27.94 0 -6 7 122.26 11.16 0 -6 7 107.49 15.04 0 -6 7 117.34 10.83 0 -6 7 121.12 16.14 0 -6 8 14.60 4.49 0 -6 8 21.75 7.81 0 -6 8 19.65 7.62 0 -6 8 18.44 4.48 0 -6 9 103.73 9.39 0 -6 9 114.09 14.18 0 -6 9 93.69 11.77 0 -6 10 186.30 11.83 0 -6 10 172.14 16.28 0 -6 11 242.05 13.79 0 -6 11 228.26 17.74 0 -6 12 7.09 1.84 0 -5 0 -2.65 5.63 0 -5 0 3.79 8.05 0 -5 0 2.27 5.90 0 -5 0 0.58 3.09 0 -5 0 11.94 5.96 0 -5 0 1.08 5.14 0 -5 0 2.45 3.84 0 -5 -1 746.46 78.88 0 -5 1 760.93 66.89 0 -5 -1 942.24 72.60 0 -5 1 723.95 72.90 0 -5 -1 922.48 53.65 0 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87.08 26.58 0 3 -11 79.36 9.28 0 3 -11 77.33 17.80 0 3 -11 81.93 9.41 0 3 -11 95.36 9.97 0 3 -11 90.33 9.66 0 3 -11 84.93 9.32 0 3 -11 88.15 10.87 0 3 -12 383.52 23.45 0 3 12 307.43 43.62 0 3 -12 392.67 23.98 0 3 -12 384.37 23.83 0 3 -12 309.67 37.38 0 3 -12 328.27 37.92 0 3 12 337.36 54.28 0 3 -12 382.17 23.47 0 3 -12 364.82 22.70 0 3 -12 405.69 23.79 0 3 -12 394.97 23.89 0 3 -12 409.20 25.98 0 3 -12 373.79 22.95 0 3 -12 383.79 23.52 0 3 -13 207.79 15.07 0 3 -13 171.70 14.24 0 3 -13 175.22 14.48 0 3 -13 164.18 13.42 0 3 -13 209.30 15.56 0 3 -13 190.09 14.37 0 3 -13 191.59 16.46 0 3 -13 203.30 15.14 0 3 -13 210.70 15.75 0 3 -13 199.70 15.35 0 3 -14 996.02 48.67 0 3 -14 1063.24 50.03 0 3 -14 1048.61 50.00 0 3 -14 995.00 48.97 0 3 -14 1090.62 50.00 0 3 -14 1073.95 52.32 0 3 -14 1003.73 48.18 0 3 -14 1048.75 49.92 0 3 -15 41.64 6.03 0 3 -15 33.25 5.80 0 3 -15 43.94 7.60 0 3 -15 44.75 6.55 0 3 -16 56.55 6.73 0 3 -16 50.00 6.38 0 3 -16 63.00 7.87 0 3 -17 45.52 5.21 0 3 -17 37.80 4.83 0 3 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835.72 41.23 -1 2 -11 789.62 40.50 -1 2 -11 794.87 40.59 -1 2 -11 833.07 41.25 -1 2 -11 851.68 43.74 -1 2 -11 818.45 40.74 -1 2 -12 107.08 10.58 1 2 12 108.86 24.73 1 2 12 69.19 24.96 1 2 12 65.45 20.63 -1 2 -12 85.48 17.50 -1 2 -12 79.78 9.02 -1 2 -12 95.87 10.08 -1 2 -12 105.74 10.51 -1 2 -12 101.35 10.30 -1 2 -12 94.75 9.82 -1 2 -12 118.14 10.80 -1 2 -12 117.96 12.25 1 2 13 465.68 54.92 -1 2 -13 524.41 29.29 1 2 13 453.78 64.59 -1 2 -13 480.37 27.50 1 2 13 392.45 53.05 -1 2 -13 547.67 32.10 -1 2 -13 510.05 28.74 -1 2 -13 530.80 29.43 -1 2 -13 591.56 30.40 -1 2 -13 519.31 28.68 -1 2 -14 193.26 16.97 -1 2 -14 189.68 14.48 -1 2 -14 187.60 14.10 -1 2 -14 216.41 15.91 -1 2 -14 207.21 15.41 -1 2 -15 315.38 21.58 -1 2 -15 288.41 19.18 -1 2 -15 279.77 17.93 -1 2 -15 299.19 19.42 -1 2 -16 452.76 25.14 -1 2 -16 440.61 26.74 -1 2 -16 450.27 25.18 -1 2 -17 83.19 7.80 -1 2 -17 88.84 8.13 -1 2 -17 90.24 8.43 -1 2 -18 62.02 5.67 -1 2 -18 74.39 6.68 -1 2 -18 77.97 6.59 1 3 -18 113.59 7.54 1 3 -18 99.76 7.78 1 3 -17 83.59 7.39 1 3 -17 77.98 7.92 1 3 -16 30.90 5.27 1 3 -16 31.57 5.92 1 3 -16 27.18 4.68 1 3 -15 268.05 17.60 1 3 -15 273.05 19.13 1 3 -15 264.64 17.15 1 3 -14 117.55 11.18 1 3 -14 104.52 10.00 1 3 -14 125.86 11.57 1 3 -14 125.75 12.69 1 3 -14 106.41 10.44 1 3 -14 110.96 10.64 1 3 -14 114.74 11.01 1 3 -13 1042.90 49.46 1 3 -13 1003.03 50.65 1 3 -13 1067.35 50.74 1 3 -13 1109.88 51.68 1 3 -13 1011.68 49.58 1 3 -13 1104.47 51.27 1 3 -13 1088.92 53.41 1 3 -13 974.41 48.44 1 3 -13 1077.52 50.90 1 3 -13 1087.85 51.43 1 3 -12 84.18 9.22 -1 3 12 52.10 17.35 1 3 -12 88.58 9.75 -1 3 12 109.01 32.64 1 3 -12 69.60 17.98 1 3 -12 82.48 9.42 1 3 -12 89.38 9.77 1 3 -12 89.97 9.93 1 3 -12 84.47 9.34 1 3 -12 94.53 11.05 1 3 -12 91.87 9.91 -1 3 11 124.07 25.32 1 3 -11 171.21 14.05 1 3 -11 188.28 31.16 -1 3 11 168.96 38.67 1 3 -11 153.83 25.36 1 3 -11 163.67 25.82 1 3 -11 182.63 14.32 1 3 -11 172.52 14.04 1 3 -11 177.62 14.44 1 3 -11 176.87 14.37 1 3 -11 169.16 13.94 1 3 -11 202.78 16.44 -1 3 10 484.83 50.13 -1 3 10 583.91 70.62 1 3 -10 531.94 48.36 1 3 -10 469.08 46.61 1 3 -10 558.85 57.04 1 3 -10 561.34 30.33 1 3 -10 536.40 30.39 1 3 -10 543.69 30.32 1 3 -10 539.47 29.95 1 3 -10 598.70 32.75 1 3 -10 576.19 30.19 -1 3 9 18.69 9.93 -1 3 9 8.49 10.42 1 3 -9 4.08 5.61 1 3 -9 24.81 10.72 1 3 -9 12.71 3.85 1 3 -9 10.79 3.87 1 3 -9 6.85 3.18 1 3 -9 4.14 3.49 1 3 -9 6.62 3.09 1 3 -9 5.83 3.00 -1 3 8 1939.22 110.96 1 3 -8 1977.46 145.17 -1 3 8 1904.43 131.55 1 3 -8 1938.07 106.86 1 3 -8 1989.94 84.60 1 3 -8 1858.08 84.02 1 3 -8 1928.24 86.45 1 3 -8 1984.64 85.07 1 3 -8 1993.51 84.77 1 3 -7 1020.06 97.73 1 3 -7 1256.51 74.43 -1 3 7 1221.92 94.22 -1 3 7 1088.50 73.49 1 3 -7 1154.29 53.22 1 3 -7 1228.04 55.47 1 3 -6 274.99 44.32 1 3 -6 259.85 27.86 -1 3 6 290.00 30.32 1 3 -6 283.25 17.94 1 3 -5 10.99 11.01 1 3 -5 7.26 6.18 -1 3 5 9.96 6.05 1 3 -5 7.76 4.47 1 3 -4 787.55 73.14 -1 3 4 996.35 60.73 1 3 -4 914.76 56.26 1 3 -4 844.44 48.75 1 3 -3 212.74 34.46 1 3 -3 188.77 20.97 1 3 -3 183.38 17.22 -1 3 3 179.93 19.34 1 3 -2 2907.63 160.44 1 3 -2 2903.79 128.97 1 3 -2 2930.74 137.11 -1 3 2 2912.33 135.39 -1 3 1 548.71 47.64 -1 3 1 528.66 41.63 1 3 -1 697.06 58.74 1 3 -1 628.35 42.34 -1 3 1 592.31 36.57 1 3 -1 642.61 37.58 -1 3 0 150.33 21.16 -1 3 0 118.60 18.30 1 3 0 159.17 25.83 1 3 0 171.57 17.22 1 3 0 190.45 20.64 -1 3 0 136.86 14.73 -1 3 -1 421.36 34.97 -1 3 -1 596.67 59.30 -1 3 -1 526.35 40.86 1 3 1 486.18 45.79 1 3 1 441.78 32.89 -1 3 -1 551.54 32.77 1 3 2 346.33 38.09 1 3 2 379.47 35.72 -1 3 -2 417.83 50.53 1 3 2 324.79 28.53 -1 3 -2 383.52 27.02 -1 3 -2 417.97 36.67 -1 3 -3 2690.63 155.33 1 3 3 2492.18 123.42 1 3 3 2275.55 117.06 -1 3 -3 2370.47 110.92 -1 3 -3 2489.33 126.22 1 3 4 1359.92 76.46 -1 3 -4 1456.13 109.65 -1 3 -4 1502.47 86.57 1 3 4 1385.25 82.13 -1 3 -4 1312.47 70.92 1 3 5 304.22 28.66 -1 3 -5 252.47 43.91 1 3 5 279.77 32.34 -1 3 -5 222.03 22.70 -1 3 -5 236.37 30.12 -1 3 -6 143.83 34.33 -1 3 -6 104.82 15.81 1 3 6 135.44 24.35 1 3 6 131.85 19.33 -1 3 -6 117.84 10.69 -1 3 -6 132.53 9.74 1 3 7 196.66 25.55 -1 3 -7 284.65 16.94 -1 3 -7 282.36 49.58 -1 3 -7 275.62 27.32 1 3 7 268.59 36.71 -1 3 -7 291.28 33.98 -1 3 -7 254.26 15.85 -1 3 -7 280.85 16.73 -1 3 -7 252.01 15.87 -1 3 -7 267.99 15.82 -1 3 -7 241.42 17.37 1 3 8 506.86 42.62 1 3 8 636.71 55.48 -1 3 -8 480.09 26.70 -1 3 -8 486.41 40.37 -1 3 -8 552.34 49.64 1 3 8 493.22 53.71 -1 3 -8 499.56 26.82 -1 3 -8 488.60 27.04 -1 3 -8 479.07 26.10 -1 3 -8 486.84 25.85 -1 3 -8 525.41 29.07 -1 3 -8 508.93 26.57 1 3 9 2194.88 126.28 1 3 9 1991.88 131.17 -1 3 -9 2045.99 117.87 -1 3 -9 1901.07 106.43 -1 3 -9 2030.55 87.51 -1 3 -9 1995.90 86.93 -1 3 -9 1982.08 86.12 -1 3 -9 1998.41 87.24 -1 3 -9 1956.86 86.55 -1 3 -9 1932.84 86.05 -1 3 -9 2041.84 89.51 1 3 10 111.69 25.15 -1 3 -10 70.58 8.68 -1 3 -10 74.67 16.23 -1 3 -10 77.28 29.33 -1 3 -10 86.95 9.58 -1 3 -10 85.54 9.33 -1 3 -10 82.29 18.86 -1 3 -10 69.78 8.45 -1 3 -10 83.41 9.30 -1 3 -10 76.50 8.69 -1 3 -10 91.19 10.84 -1 3 -10 78.04 8.72 -1 3 -11 293.51 19.90 1 3 11 334.30 44.72 -1 3 -11 280.59 36.23 -1 3 -11 268.63 32.05 -1 3 -11 283.46 19.61 -1 3 -11 338.49 20.42 -1 3 -11 300.64 19.20 -1 3 -11 282.73 19.42 -1 3 -11 283.60 19.28 -1 3 -11 299.67 21.53 -1 3 -11 268.39 18.46 -1 3 -11 279.56 19.53 -1 3 -11 251.35 18.71 1 3 12 250.49 40.19 -1 3 -12 307.70 20.83 -1 3 -12 228.49 32.72 -1 3 -12 303.60 20.09 -1 3 -12 338.79 21.38 -1 3 -12 320.39 20.78 -1 3 -12 316.86 20.60 -1 3 -12 300.20 20.25 -1 3 -12 320.70 20.88 -1 3 -12 334.17 20.71 -1 3 -12 314.52 20.60 -1 3 -12 308.88 22.34 -1 3 -12 329.33 21.08 -1 3 -13 20.97 5.36 -1 3 -13 16.59 4.34 -1 3 -13 27.73 5.47 -1 3 -13 25.41 5.30 -1 3 -13 23.69 5.72 -1 3 -13 33.65 6.42 -1 3 -13 27.54 5.71 -1 3 -13 25.18 6.37 -1 3 -13 23.66 5.60 -1 3 -14 466.96 26.72 -1 3 -14 448.29 26.07 -1 3 -14 479.92 27.22 -1 3 -14 504.34 29.37 -1 3 -14 473.56 26.53 -1 3 -14 524.92 27.62 -1 3 -14 470.57 26.10 -1 3 -15 322.60 19.27 -1 3 -15 292.27 17.87 -1 3 -15 291.47 20.14 -1 3 -15 317.16 18.91 -1 3 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1 4 -10 840.86 42.41 1 4 -10 863.49 43.05 1 4 -9 66.03 16.93 -1 4 9 105.19 30.70 1 4 -9 103.12 26.34 1 4 -9 107.76 10.68 1 4 -9 100.58 10.19 1 4 -9 91.07 9.44 1 4 -9 97.62 10.07 1 4 -9 96.15 11.02 1 4 -9 83.87 9.63 1 4 -9 113.23 24.09 1 4 -8 118.51 21.33 -1 4 8 113.91 30.94 1 4 -8 143.15 27.12 1 4 -8 121.62 11.07 1 4 -8 109.33 10.35 1 4 -8 120.82 11.17 1 4 -8 124.41 12.19 1 4 -8 101.62 10.68 1 4 -7 203.49 44.65 -1 4 7 162.83 36.02 1 4 -7 191.54 27.73 1 4 -7 264.72 16.99 1 4 -7 224.17 15.70 1 4 -7 220.75 16.75 1 4 -7 248.69 16.76 1 4 -6 243.09 29.09 -1 4 6 192.06 28.26 1 4 -6 225.19 15.15 1 4 -6 207.16 43.48 1 4 -5 1387.63 118.36 1 4 -5 1509.76 88.50 1 4 -4 199.47 40.00 1 4 -4 184.86 24.79 1 4 -3 673.78 72.77 1 4 -3 595.12 47.83 -1 4 3 620.07 44.54 -1 4 3 660.10 65.91 -1 4 2 113.52 19.35 1 4 -2 138.21 31.71 -1 4 2 97.92 23.17 -1 4 2 96.65 15.52 1 4 -2 161.29 22.20 -1 4 1 441.43 41.48 -1 4 1 384.26 32.43 1 4 -1 506.24 41.19 1 4 -1 426.53 54.52 1 4 0 908.33 59.75 -1 4 0 785.22 60.70 -1 4 0 722.12 48.41 -1 4 0 913.63 88.86 1 4 0 858.37 76.07 -1 4 -1 1591.99 98.49 -1 4 -1 1563.39 82.20 1 4 1 1529.69 91.28 1 4 1 1613.23 104.17 1 4 1 1650.97 111.93 -1 4 -1 1752.88 131.63 1 4 2 254.84 30.55 -1 4 -2 292.70 26.54 -1 4 -2 307.20 37.02 1 4 2 280.22 36.61 -1 4 -2 371.53 56.82 1 4 3 97.37 16.87 1 4 3 123.83 22.85 -1 4 -3 143.64 37.51 -1 4 -3 150.83 26.26 -1 4 -4 223.90 33.16 1 4 4 206.91 26.29 -1 4 -4 257.70 48.70 -1 4 -5 96.98 23.07 -1 4 -5 140.51 38.70 1 4 5 109.99 20.23 1 4 5 179.72 25.30 -1 4 -6 970.31 74.77 -1 4 -6 873.89 41.17 -1 4 -6 851.44 40.42 -1 4 -7 566.62 79.70 -1 4 -7 633.61 31.90 -1 4 -7 631.07 31.57 -1 4 -7 579.99 30.40 1 4 8 329.87 45.42 -1 4 -8 388.79 46.56 -1 4 -8 369.41 65.38 -1 4 -8 443.95 24.59 -1 4 -8 383.86 23.36 -1 4 -8 440.78 24.85 -1 4 -8 410.77 23.24 1 4 9 10.21 10.30 -1 4 -9 32.49 21.12 -1 4 -9 31.46 5.94 -1 4 -9 34.51 6.55 -1 4 -9 17.73 10.32 -1 4 -9 31.28 5.66 -1 4 -9 31.62 5.33 -1 4 -9 32.54 5.57 -1 4 -9 36.90 6.46 -1 4 -9 27.34 6.09 1 4 10 396.95 51.36 -1 4 -10 428.03 48.65 -1 4 -10 475.44 27.84 -1 4 -10 422.07 70.53 -1 4 -10 477.06 27.29 -1 4 -10 459.63 26.21 -1 4 -10 477.45 28.49 -1 4 -10 492.39 27.27 -1 4 -10 481.19 27.65 -1 4 -10 457.94 25.95 -1 4 -10 516.18 28.58 -1 4 -11 681.35 35.79 -1 4 -11 682.05 35.24 -1 4 -11 655.50 33.76 -1 4 -11 693.96 35.05 -1 4 -11 702.59 36.05 -1 4 -11 620.96 33.57 -1 4 -11 677.91 35.39 -1 4 -11 645.61 36.07 -1 4 -11 661.38 35.71 -1 4 -12 487.50 27.74 -1 4 -12 463.55 26.72 -1 4 -12 498.58 27.26 -1 4 -12 509.85 27.87 -1 4 -12 472.50 26.66 -1 4 -12 477.76 25.83 -1 4 -12 479.40 27.30 -1 4 -12 486.59 27.42 -1 4 -12 451.50 27.79 -1 4 -12 491.27 27.60 -1 4 -13 113.64 10.33 -1 4 -13 104.30 9.56 -1 4 -13 95.48 8.91 -1 4 -13 115.80 10.29 -1 4 -13 109.00 10.08 -1 4 -13 96.57 9.89 -1 4 -13 100.21 10.45 -1 4 -13 105.70 10.14 -1 4 -14 144.15 11.07 -1 4 -14 155.74 11.48 -1 4 -14 127.80 9.72 -1 4 -14 146.43 11.28 -1 4 -14 132.99 10.64 -1 4 -14 121.32 11.09 -1 4 -15 61.09 6.34 -1 4 -15 58.91 6.58 -1 4 -15 58.57 6.32 -1 4 -16 120.06 8.32 1 5 -14 2.00 1.92 1 5 -13 18.23 3.83 1 5 -13 24.71 4.12 1 5 -13 21.49 3.44 1 5 -13 26.82 4.35 1 5 -13 23.16 4.21 1 5 -12 305.61 18.27 1 5 -12 323.81 18.76 1 5 -12 344.40 19.03 1 5 -12 312.07 17.68 1 5 -12 308.28 18.23 1 5 -12 325.11 18.93 1 5 -12 292.74 17.86 1 5 -12 302.99 18.46 1 5 -11 771.14 37.79 1 5 -11 807.05 39.30 1 5 -11 802.05 39.17 1 5 -11 813.88 39.43 1 5 -11 765.79 38.45 1 5 -11 825.04 39.48 1 5 -10 112.65 10.71 1 5 -10 92.85 9.89 1 5 -10 107.68 9.73 1 5 -10 101.23 9.61 1 5 -10 112.22 10.28 1 5 -10 117.57 10.84 1 5 -9 120.92 11.23 1 5 -9 114.73 10.35 1 5 -9 123.73 11.20 1 5 -9 110.01 10.35 1 5 -9 116.15 11.19 1 5 -8 8.72 3.97 1 5 -8 10.78 3.56 1 5 -8 6.81 3.54 1 5 -8 13.71 3.91 1 5 -7 121.93 10.87 1 5 -7 105.10 10.49 1 5 -7 126.91 11.56 1 5 -6 927.84 68.48 1 5 -6 911.50 79.15 1 5 -6 974.72 46.25 1 5 -6 1013.99 47.08 1 5 -6 807.87 84.51 1 5 -5 187.65 38.57 1 5 -5 191.08 27.58 -1 5 4 168.49 42.35 1 5 -4 258.22 44.29 1 5 -4 208.39 28.78 1 5 -3 356.96 51.58 -1 5 3 353.32 60.08 1 5 -3 311.23 36.10 1 5 -2 20.30 13.19 -1 5 2 29.80 20.69 1 5 -2 13.31 9.05 1 5 -1 946.76 85.00 -1 5 1 946.80 103.01 1 5 -1 908.65 67.35 1 5 0 266.17 42.18 -1 5 0 336.29 59.71 -1 5 0 371.14 42.95 1 5 0 259.52 33.77 -1 5 -1 148.05 27.42 -1 5 -1 99.36 33.60 1 5 1 124.58 27.66 1 5 1 142.09 24.95 -1 5 -2 789.63 94.40 -1 5 -2 653.96 63.94 1 5 2 769.73 60.79 -1 5 -3 -3.21 6.81 -1 5 -3 6.43 13.67 1 5 3 12.25 7.95 -1 5 -4 13.12 10.65 1 5 4 7.55 8.17 -1 5 -4 -6.57 8.06 -1 5 -5 485.44 75.64 -1 5 -5 543.70 28.13 -1 5 -5 544.52 58.04 1 5 5 371.57 44.86 -1 5 -6 76.22 20.91 -1 5 -6 66.76 7.88 -1 5 -6 60.07 28.49 -1 5 -6 76.73 8.66 1 5 6 65.46 17.51 -1 5 -7 653.77 34.03 -1 5 -7 621.65 32.77 -1 5 -7 631.94 33.32 -1 5 -8 241.85 16.77 -1 5 -8 266.81 18.13 -1 5 -8 271.27 17.82 -1 5 -8 269.05 18.40 -1 5 -9 11.32 4.71 -1 5 -9 14.81 3.82 -1 5 -9 12.45 4.22 -1 5 -9 17.13 4.71 -1 5 -9 14.09 4.11 -1 5 -10 43.82 7.04 -1 5 -10 45.21 6.74 -1 5 -10 31.21 5.46 -1 5 -10 40.14 6.26 -1 5 -10 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169.83 13.61 7 4 -4 179.65 13.42 7 4 -4 198.92 13.82 7 4 -3 274.74 17.98 7 4 -3 285.22 18.11 7 4 -2 19.65 4.95 -7 4 2 27.08 5.37 7 4 -2 30.30 5.72 7 4 -1 315.49 20.28 -7 4 1 338.83 21.34 7 4 -1 339.26 20.65 7 4 0 127.65 11.40 -7 4 0 136.41 12.51 7 4 0 125.88 11.22 7 4 0 123.44 11.38 7 4 1 200.30 14.56 -7 4 -1 162.63 12.48 -7 4 -1 181.74 15.02 7 4 1 181.32 13.78 7 4 1 181.67 13.87 7 4 2 83.40 9.01 -7 4 -2 61.05 7.48 -7 4 -2 67.04 8.92 -7 4 -3 51.92 6.99 -7 4 -3 73.92 9.27 -7 4 -4 145.40 11.85 -7 4 -4 148.76 12.93 -7 4 -5 241.62 14.97 -7 4 -5 257.58 16.63 -7 4 -5 297.57 18.37 -7 4 -6 106.20 8.53 -7 4 -6 120.51 9.81 -7 4 -7 38.63 5.11 -7 4 -7 36.07 5.18 -7 4 -8 73.89 6.50 7 5 -5 29.31 3.50 7 5 -5 25.33 3.41 7 5 -4 6.94 2.19 7 5 -3 86.35 7.14 7 5 -2 280.11 15.66 7 5 -1 14.61 2.93 7 5 -1 18.41 3.44 7 5 -1 15.34 2.80 7 5 0 88.97 7.17 7 5 0 100.93 7.76 7 5 1 2.67 1.68 7 5 1 4.29 2.25 7 5 1 6.82 2.01 7 5 2 2.58 1.79 -7 5 -2 4.64 2.31 7 5 3 131.66 8.86 8 -4 -6 124.13 10.25 8 -4 -5 44.85 6.66 -8 -4 5 36.34 6.09 -8 -4 5 32.88 4.14 -8 -4 4 181.15 11.39 -8 -4 3 38.90 4.94 -8 -4 2 56.19 6.31 -8 -4 2 51.61 5.97 8 -4 -2 48.20 8.07 -8 -4 1 119.10 9.95 -8 -4 1 119.20 9.25 8 -4 -1 116.59 12.48 -8 -4 0 155.36 11.61 8 -4 0 143.29 13.84 -8 -4 -1 58.27 6.81 8 -4 1 57.67 8.25 8 -4 2 19.29 4.89 -8 -4 -2 22.49 4.04 -8 -4 -2 25.87 4.64 -8 -4 -3 156.15 9.93 -8 -4 -3 110.80 9.47 -8 -4 -4 17.67 3.16 8 -3 -9 166.88 11.71 -8 -3 8 137.25 9.04 -8 -3 8 143.65 11.36 8 -3 -8 119.45 10.71 -8 -3 7 61.54 6.21 8 -3 -7 54.59 7.67 -8 -3 6 67.09 6.92 8 -3 -6 66.89 8.39 -8 -3 5 319.50 18.66 8 -3 -4 36.80 9.17 -8 -3 4 34.46 5.52 -8 -3 4 39.40 5.81 -8 -3 3 399.16 23.38 8 -3 -3 458.04 30.46 -8 -3 3 394.29 22.70 8 -3 -2 49.09 10.23 -8 -3 2 51.01 6.76 8 -3 -1 46.64 10.22 -8 -3 1 28.64 5.24 8 -3 0 198.12 18.26 -8 -3 0 139.34 11.59 8 -3 1 82.98 11.91 -8 -3 -1 76.90 7.92 8 -3 2 171.81 16.88 -8 -3 -2 214.66 14.94 8 -3 3 120.00 12.85 -8 -3 -3 147.56 11.79 8 -3 4 16.76 4.86 -8 -3 -4 26.08 4.89 -8 -3 -5 41.29 5.61 -8 -3 -6 161.29 11.06 -8 -3 -7 23.29 3.98 -8 -3 -7 21.84 3.49 -8 -3 -8 228.33 12.53 8 -2 -11 23.34 4.16 8 -2 -10 424.69 21.74 -8 -2 10 430.15 23.67 8 -2 -9 135.56 11.96 -8 -2 9 155.50 13.67 8 -2 -8 42.23 7.06 -8 -2 8 49.63 8.31 8 -2 -7 16.41 5.13 -8 -2 7 21.73 6.26 8 -2 -6 59.78 8.75 -8 -2 6 87.21 11.41 -8 -2 5 62.69 10.04 8 -2 -5 50.16 8.29 8 -2 -5 59.52 8.07 -8 -2 5 49.72 8.64 -8 -2 4 1285.30 58.25 8 -2 -4 898.21 51.63 8 -2 -4 1108.02 52.13 -8 -2 4 1073.95 54.35 -8 -2 3 37.56 8.64 8 -2 -3 34.83 7.28 -8 -2 3 44.04 8.15 8 -2 -3 39.87 7.14 -8 -2 2 150.59 15.80 -8 -2 2 144.73 14.67 -8 -2 2 122.78 12.78 8 -2 -2 154.31 13.64 -8 -2 1 45.72 8.75 -8 -2 1 31.59 7.49 -8 -2 1 29.24 6.61 8 -2 -1 34.78 6.79 8 -2 0 163.60 18.11 -8 -2 0 159.92 15.38 -8 -2 0 175.97 15.50 8 -2 0 158.93 14.24 8 -2 1 914.66 49.09 -8 -2 -1 827.34 44.77 8 -2 1 773.03 42.46 -8 -2 -1 896.61 45.00 8 -2 2 297.37 23.91 -8 -2 -2 350.38 23.08 8 -2 2 323.35 21.55 8 -2 3 12.55 5.77 -8 -2 -3 17.84 5.46 8 -2 3 15.58 4.83 -8 -2 -3 25.13 5.38 -8 -2 -4 152.41 12.51 -8 -2 -5 27.39 5.15 -8 -2 -6 128.14 11.36 -8 -2 -6 116.69 9.85 -8 -2 -7 246.87 15.67 -8 -2 -7 221.08 13.85 -8 -2 -8 5.20 2.49 -8 -2 -8 2.37 1.68 -8 -2 -9 67.15 6.33 8 -1 -12 117.77 9.39 8 -1 -12 143.60 9.48 8 -1 -11 123.39 9.73 8 -1 -11 101.01 9.56 8 -1 -10 12.77 4.33 8 -1 -9 130.81 12.25 8 -1 -8 116.39 11.92 8 -1 -7 499.97 28.28 8 -1 -7 411.12 27.08 8 -1 -6 152.69 14.13 8 -1 -6 140.02 13.65 8 -1 -5 308.16 21.35 8 -1 -5 249.92 19.44 8 -1 -4 109.54 12.03 8 -1 -4 73.78 9.79 -8 -1 3 172.83 14.37 8 -1 -3 190.58 16.31 -8 -1 2 359.18 27.17 8 -1 -2 407.14 26.04 -8 -1 2 331.68 23.09 -8 -1 1 277.97 23.17 8 -1 -1 315.98 21.98 -8 -1 1 253.43 19.79 -8 -1 0 59.36 10.32 8 -1 0 60.40 8.98 -8 -1 0 79.41 10.28 -8 -1 -1 123.28 14.65 -8 -1 -1 128.64 13.22 8 -1 1 118.10 13.10 8 -1 2 108.25 13.25 -8 -1 -2 95.08 13.37 8 -1 2 104.07 12.26 -8 -1 -2 122.83 12.80 -8 -1 -3 113.39 10.56 -8 -1 -3 117.30 13.89 8 -1 3 125.43 13.19 -8 -1 -3 89.78 11.66 -8 -1 -4 477.87 26.46 8 -1 4 500.94 30.35 -8 -1 -4 514.56 30.50 8 -1 5 101.77 11.59 -8 -1 -5 104.74 11.57 8 -1 6 201.42 16.37 8 -1 7 14.66 5.08 -8 -1 -7 19.57 5.02 8 -1 8 221.00 16.03 -8 -1 -8 222.44 15.24 -8 -1 -9 99.94 8.43 8 -1 9 109.70 9.71 -8 -1 -9 99.82 8.56 8 -1 10 107.33 8.66 -8 -1 -10 107.64 7.41 -8 0 13 136.43 10.17 -8 0 12 77.51 8.79 8 0 -12 67.10 6.69 -8 0 11 381.12 23.50 8 0 -11 372.53 19.53 -8 0 10 6.59 4.92 8 0 -10 3.79 3.24 -8 0 9 55.07 9.89 8 0 -9 42.90 6.96 -8 0 8 402.38 27.59 8 0 -8 361.40 23.22 -8 0 7 -1.89 5.18 8 0 -7 3.50 3.43 8 0 -7 1.35 3.80 -8 0 6 545.71 34.46 8 0 -6 555.12 31.17 -8 0 5 121.25 15.22 8 0 -5 113.30 12.94 -8 0 4 6.99 6.62 8 0 -4 22.58 6.55 -8 0 3 329.77 27.04 8 0 -3 340.75 24.26 -8 0 2 169.81 17.98 -8 0 2 162.70 17.60 -8 0 2 157.49 13.83 8 0 -2 164.01 15.75 -8 0 1 379.12 28.51 -8 0 1 362.46 28.11 -8 0 1 369.37 24.08 8 0 -1 381.58 26.18 -8 0 0 616.18 39.07 -8 0 0 599.13 38.72 8 0 0 649.99 36.92 -8 0 0 611.80 34.83 -8 0 0 587.26 34.13 -8 0 -1 13.20 6.89 8 0 1 16.97 6.25 -8 0 -1 29.04 6.67 -8 0 -2 107.38 13.83 8 0 2 94.31 12.28 -8 0 -2 108.96 11.88 -8 0 -3 476.29 32.60 8 0 3 495.17 31.25 -8 0 -3 504.07 29.91 8 0 4 -0.74 4.06 -8 0 -4 4.46 4.21 8 0 5 770.40 41.94 -8 0 -5 757.26 40.09 8 0 6 346.60 23.62 8 0 7 36.97 7.40 -8 0 -7 37.78 6.22 8 0 8 100.87 10.87 -8 0 -8 99.04 9.22 8 0 9 17.26 4.79 8 0 10 61.32 6.96 -8 0 -10 53.99 5.78 -8 1 12 98.30 8.58 -8 1 11 128.10 11.25 8 1 -11 81.50 7.23 -8 1 10 20.40 5.81 8 1 -10 14.17 3.37 -8 1 9 154.85 14.92 8 1 -9 142.06 11.26 -8 1 8 152.14 15.39 8 1 -8 125.09 11.21 -8 1 7 496.95 32.55 8 1 -7 515.59 30.11 -8 1 6 162.22 16.96 8 1 -6 164.47 14.97 -8 1 5 341.95 25.87 8 1 -5 338.95 23.62 -8 1 4 97.53 13.45 8 1 -4 101.41 12.14 8 1 -4 96.74 9.56 -8 1 3 216.88 19.91 8 1 -3 202.85 17.45 8 1 -3 196.52 14.76 8 1 -2 394.09 23.12 -8 1 2 410.81 28.81 8 1 -2 395.49 26.49 8 1 -2 366.18 22.83 -8 1 2 425.32 30.09 8 1 -1 299.93 19.67 -8 1 1 369.79 26.13 -8 1 1 343.64 21.21 8 1 -1 291.46 19.49 -8 1 1 314.93 20.80 -8 1 1 351.10 26.24 8 1 -1 293.78 22.43 8 1 0 62.55 7.92 8 1 0 64.15 7.84 -8 1 0 62.53 8.73 -8 1 0 68.17 10.99 8 1 0 80.71 10.45 8 1 1 117.45 10.86 -8 1 -1 119.23 12.10 -8 1 -1 116.48 14.43 8 1 1 139.17 14.12 8 1 2 89.88 9.24 -8 1 -2 95.10 11.01 -8 1 -2 96.20 12.92 8 1 2 79.61 11.11 -8 1 -3 124.40 12.44 -8 1 -3 107.80 13.73 8 1 3 123.71 13.50 8 1 4 507.00 31.10 -8 1 -4 516.59 30.04 8 1 5 113.79 12.47 -8 1 -5 110.39 11.45 8 1 6 171.00 15.22 -8 1 -6 177.23 14.30 8 1 7 19.07 5.54 8 1 8 206.91 15.87 -8 1 -8 229.83 14.94 8 1 9 91.19 9.20 -8 1 -9 114.89 8.87 8 1 10 92.70 8.07 8 2 -11 33.45 3.79 8 2 -11 35.50 4.14 8 2 -10 421.39 21.92 8 2 -9 169.19 12.25 8 2 -8 57.79 7.18 8 2 -7 22.51 5.17 8 2 -6 78.82 7.80 -8 2 6 55.17 8.28 8 2 -6 79.78 9.15 -8 2 5 55.42 8.37 8 2 -5 47.08 7.61 8 2 -5 52.34 6.69 8 2 -5 51.08 6.91 -8 2 5 42.38 8.51 -8 2 4 1098.44 55.53 8 2 -4 1161.35 55.18 8 2 -4 1128.55 51.92 8 2 -4 1138.04 53.11 -8 2 4 1139.87 58.20 8 2 -3 28.48 5.09 8 2 -3 27.00 5.55 -8 2 3 38.52 7.39 8 2 -3 30.27 5.83 -8 2 3 49.50 8.93 8 2 -3 26.51 6.31 8 2 -2 145.04 12.24 8 2 -2 139.10 12.11 -8 2 2 126.31 14.52 8 2 -2 141.55 13.48 8 2 -1 31.31 6.15 -8 2 1 29.86 5.44 8 2 -1 39.31 6.34 -8 2 1 35.21 8.02 8 2 -1 34.67 6.95 8 2 0 173.24 13.69 8 2 0 166.98 13.41 -8 2 0 148.13 12.95 -8 2 0 178.66 16.54 8 2 0 157.55 14.42 8 2 1 871.76 41.85 8 2 1 812.54 40.89 -8 2 -1 785.08 41.31 -8 2 -1 820.52 45.08 8 2 1 852.31 43.18 -8 2 -2 286.61 19.84 8 2 2 295.31 19.09 -8 2 -2 344.34 23.45 8 2 2 293.74 20.65 8 2 3 22.14 5.48 8 2 3 27.47 5.21 -8 2 -3 25.61 5.84 8 2 4 138.73 12.69 -8 2 -4 146.42 12.80 8 2 5 18.44 4.87 -8 2 -5 30.27 5.80 8 2 6 107.81 10.51 -8 2 -6 139.95 11.51 8 2 7 182.13 13.88 -8 2 -7 266.20 15.64 8 2 8 -3.44 3.16 -8 2 -9 51.45 5.23 8 3 -9 223.62 13.33 8 3 -8 183.56 12.39 8 3 -7 93.14 8.77 8 3 -6 94.25 9.29 8 3 -6 88.22 7.86 8 3 -5 312.21 18.08 8 3 -4 38.09 5.40 8 3 -3 389.75 21.68 8 3 -2 64.34 7.21 8 3 -1 42.64 6.33 8 3 -1 35.51 5.35 8 3 0 183.16 13.43 8 3 0 164.21 12.18 8 3 1 68.92 7.99 -8 3 -1 74.73 7.61 8 3 2 186.36 13.20 -8 3 -2 154.31 12.18 8 3 2 186.32 13.45 -8 3 -3 124.53 10.52 8 3 3 130.92 10.59 8 3 3 122.44 10.50 8 3 4 28.23 4.74 -8 3 -4 22.16 4.53 -8 3 -5 55.74 6.46 8 3 5 47.50 5.74 -8 3 -6 158.25 11.16 -8 3 -7 23.11 3.66 8 4 -5 43.19 4.59 8 4 -4 168.09 10.59 8 4 -3 37.12 4.62 8 4 -3 41.28 4.79 8 4 -3 34.96 4.52 8 4 -2 46.29 5.35 8 4 -2 44.61 4.89 8 4 -2 39.69 4.87 8 4 -2 43.17 5.13 8 4 -1 130.43 9.60 8 4 -1 134.62 9.43 8 4 -1 134.31 9.73 8 4 0 130.56 9.80 8 4 0 138.89 9.62 8 4 0 151.13 10.18 8 4 1 57.49 5.97 8 4 1 56.97 5.53 8 4 1 50.34 5.62 8 4 2 21.00 3.53 8 4 3 115.93 8.38 9 -3 -5 130.12 10.23 9 -3 -4 41.61 6.00 9 -3 -3 85.88 8.89 9 -3 -2 121.84 10.74 -9 -3 1 37.49 4.50 9 -3 -1 22.88 4.83 -9 -3 0 15.33 2.98 9 -3 0 8.59 3.08 -9 -3 -1 72.23 6.00 9 -2 -7 112.13 10.31 -9 -2 7 88.06 8.14 9 -2 -6 82.28 9.70 -9 -2 6 81.19 8.37 9 -2 -5 9.12 4.61 9 -2 -4 435.35 27.04 9 -2 -3 327.13 22.55 9 -2 -2 66.81 9.60 9 -2 -1 17.40 5.45 -9 -2 0 45.90 5.62 9 -2 0 37.55 6.69 -9 -2 -1 38.44 4.96 9 -2 1 24.58 5.14 -9 -2 -2 279.88 15.47 -9 -2 -3 56.56 5.23 -9 -2 -3 59.90 6.66 -9 -2 -4 72.18 7.01 -9 -1 9 1.62 2.10 -9 -1 8 117.09 10.24 -9 -1 7 173.45 13.71 -9 -1 6 199.53 15.47 9 -1 -5 219.93 15.23 -9 -1 5 215.88 16.68 9 -1 -4 76.26 8.66 -9 -1 4 83.58 10.37 9 -1 -3 120.51 11.01 -9 -1 3 111.25 12.13 9 -1 -2 153.43 12.62 -9 -1 2 126.31 12.91 9 -1 -1 311.22 21.66 9 -1 -1 362.11 20.95 -9 -1 1 319.54 21.63 9 -1 0 102.20 11.15 9 -1 0 129.46 11.48 -9 -1 0 141.05 13.09 -9 -1 0 111.23 10.26 9 -1 1 108.16 10.71 -9 -1 -1 115.96 11.91 -9 -1 -1 108.04 10.15 -9 -1 -2 10.53 3.77 9 -1 2 1.95 3.17 -9 -1 -3 212.82 14.96 9 -1 3 220.60 15.35 -9 -1 -4 185.22 13.68 9 -1 4 218.64 14.53 -9 -1 -5 265.82 16.39 9 -1 5 281.38 16.82 -9 -1 -6 15.21 3.34 9 -1 6 6.36 2.84 -9 0 9 23.82 4.64 -9 0 9 27.03 5.22 -9 0 8 95.57 9.77 -9 0 8 88.24 9.73 -9 0 7 400.14 24.23 -9 0 7 376.63 24.18 -9 0 6 13.17 5.22 9 0 -6 2.35 3.21 -9 0 6 1.92 4.23 -9 0 5 362.76 23.98 9 0 -5 346.15 21.59 -9 0 5 349.11 23.85 -9 0 4 49.29 8.67 9 0 -4 47.10 7.37 -9 0 4 45.18 8.28 -9 0 3 66.61 9.76 -9 0 3 58.30 9.34 9 0 -3 64.50 8.38 -9 0 2 171.31 16.35 9 0 -2 201.26 15.38 9 0 -1 39.03 6.47 -9 0 1 50.81 8.55 -9 0 1 33.24 5.16 9 0 0 418.96 25.01 -9 0 0 367.98 22.25 9 0 1 158.62 13.58 -9 0 -1 174.14 15.36 -9 0 -1 145.02 12.02 9 0 2 6.54 4.18 -9 0 -2 8.17 3.35 9 0 3 41.56 6.86 -9 0 -3 43.18 6.28 9 0 4 111.58 10.66 -9 0 -4 115.52 10.13 9 0 5 146.68 11.79 -9 0 -5 134.64 10.76 9 0 6 53.03 6.68 -9 0 -6 59.93 6.50 9 0 7 30.80 4.62 -9 0 -7 33.27 4.21 -9 1 9 6.12 2.87 -9 1 8 106.09 9.15 -9 1 8 123.44 10.71 -9 1 7 156.65 12.48 -9 1 7 182.84 14.33 -9 1 6 193.08 14.76 -9 1 6 199.69 15.90 -9 1 5 212.98 15.84 -9 1 5 205.60 16.63 9 1 -5 197.88 14.56 -9 1 4 62.42 9.35 9 1 -4 71.67 8.53 -9 1 3 116.27 12.22 9 1 -3 88.11 9.80 -9 1 2 162.09 14.49 9 1 -2 129.54 12.00 -9 1 1 331.43 22.99 9 1 -1 337.29 21.40 -9 1 0 157.41 14.32 9 1 0 133.34 12.31 -9 1 -1 112.34 11.84 9 1 1 122.28 11.09 -9 1 -2 7.18 2.99 9 1 2 12.04 4.45 -9 1 -3 196.45 13.50 9 1 3 203.24 14.81 -9 1 -4 193.59 13.30 9 1 4 206.53 14.41 -9 1 -5 258.46 15.60 9 1 5 261.55 16.35 -9 1 -6 6.17 2.25 9 1 6 12.46 3.31 9 2 -7 83.64 6.78 9 2 -6 85.24 7.03 -9 2 6 41.32 5.64 9 2 -5 10.23 3.20 -9 2 5 7.15 3.17 -9 2 4 362.45 21.36 -9 2 3 316.76 18.96 9 2 -3 263.38 16.55 -9 2 2 59.50 7.53 9 2 -2 47.40 6.23 -9 2 1 15.37 4.56 9 2 -1 11.82 3.83 9 2 0 44.54 5.98 9 2 1 25.96 4.65 9 2 2 244.13 14.81 -9 2 -3 73.33 6.61 -9 2 -4 47.81 5.16 9 3 -1 28.56 3.65 9 3 0 9.18 2.19 0 0 0 0.00 0.00 TITL songxh_210301 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 7.962947 6.035215 16.020955 90.0000 93.6369 90.0000 ZERR 3.00 0.000124 0.000099 0.000235 0.0000 0.0014 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 41855 _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 2.032 _oxdiff_exptl_absorpt_empirical_full_min 0.583 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Br10 Br 1.07213(7) 0.70832(9) 0.90430(3) 0.02814(14) Uani 1 1 d . . . . . Br9 Br 1.17197(7) 0.90858(10) 0.73036(3) 0.03012(15) Uani 1 1 d . . . . . O19 O 0.4639(5) 0.0913(7) 0.9315(2) 0.0297(8) Uani 1 1 d . . . . . O11 O 0.6916(5) 0.7053(9) 0.4054(2) 0.0355(9) Uani 1 1 d . . . . . C16 C 0.5569(6) 0.2301(10) 0.8863(3) 0.0254(11) Uani 1 1 d . . . . . C17 C 0.7172(7) 0.1520(9) 0.8687(3) 0.0284(12) Uani 1 1 d . . . . . H17 H 0.752641 0.012214 0.886699 0.034 Uiso 1 1 calc R U . . . C18 C 0.8217(7) 0.2844(9) 0.8243(3) 0.0269(12) Uani 1 1 d . . . . . H18 H 0.927458 0.231814 0.812575 0.032 Uiso 1 1 calc R U . . . C8 C 1.0201(6) 0.7310(10) 0.7870(3) 0.0264(11) Uani 1 1 d . . . . . C2 C 0.8880(7) 0.5062(11) 0.6010(3) 0.0280(11) Uani 1 1 d . . . . . H2 H 0.953068 0.385818 0.619499 0.034 Uiso 1 1 calc R U . . . C7 C 0.8858(6) 0.6372(9) 0.7493(3) 0.0226(10) Uani 1 1 d . . . . . C4 C 0.7383(6) 0.7048(12) 0.4887(3) 0.0271(10) Uani 1 1 d . . . . . C13 C 0.7722(6) 0.4940(10) 0.7969(3) 0.0226(10) Uani 1 1 d . . . . . C1 C 0.8414(6) 0.6659(9) 0.6580(3) 0.0245(11) Uani 1 1 d . . . . . C15 C 0.5046(7) 0.4387(10) 0.8581(3) 0.0259(12) Uani 1 1 d . . . . . H15 H 0.398578 0.491151 0.869433 0.031 Uiso 1 1 calc R U . . . C5 C 0.6924(7) 0.8650(10) 0.5453(3) 0.0294(12) Uani 1 1 d . . . . . H5 H 0.627351 0.985737 0.527051 0.035 Uiso 1 1 calc R U . . . C3 C 0.8380(7) 0.5260(11) 0.5169(3) 0.0309(12) Uani 1 1 d . . . . . H3 H 0.870890 0.419973 0.479052 0.037 Uiso 1 1 calc R U . . . C20 C 0.3109(7) 0.1792(11) 0.9604(3) 0.0303(12) Uani 1 1 d . . . . . H20A H 0.230620 0.199091 0.913745 0.045 Uiso 1 1 calc R U . . . H20B H 0.333306 0.319279 0.987200 0.045 Uiso 1 1 calc R U . . . H20C H 0.266364 0.077994 0.999604 0.045 Uiso 1 1 calc R U . . . C14 C 0.6110(6) 0.5683(9) 0.8130(3) 0.0245(11) Uani 1 1 d . . . . . H14 H 0.574598 0.706181 0.793210 0.029 Uiso 1 1 calc R U . . . C6 C 0.7445(8) 0.8433(10) 0.6293(4) 0.0326(13) Uani 1 1 d . . . . . H6 H 0.713383 0.950553 0.667091 0.039 Uiso 1 1 calc R U . . . C12 C 0.5908(9) 0.8871(15) 0.3738(4) 0.0491(18) Uani 1 1 d . . . . . H12A H 0.564243 0.866858 0.315003 0.074 Uiso 1 1 calc R U . . . H12B H 0.652084 1.022912 0.382737 0.074 Uiso 1 1 calc R U . . . H12C H 0.488683 0.893229 0.402461 0.074 Uiso 1 1 calc R U . . . 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 Br10 0.0268(3) 0.0341(3) 0.0234(2) -0.0015(2) 0.00056(19) 0.0006(2) Br9 0.0265(3) 0.0343(3) 0.0304(3) -0.0007(2) 0.0089(2) -0.0031(3) O19 0.0287(19) 0.031(2) 0.0303(19) 0.0049(16) 0.0091(16) 0.0012(17) O11 0.041(2) 0.046(2) 0.0201(16) 0.001(2) 0.0025(15) 0.014(2) C16 0.030(3) 0.028(3) 0.018(2) 0.000(2) 0.0034(19) -0.001(2) C17 0.033(3) 0.024(3) 0.028(3) 0.003(2) 0.004(2) 0.005(2) C18 0.028(3) 0.027(3) 0.026(3) 0.001(2) 0.008(2) 0.006(2) C8 0.027(3) 0.026(3) 0.027(2) -0.003(2) 0.0037(19) 0.001(2) C2 0.029(3) 0.032(3) 0.024(2) 0.002(2) 0.002(2) 0.007(2) C7 0.025(2) 0.020(3) 0.023(2) -0.0009(18) 0.0047(19) 0.0048(19) C4 0.026(2) 0.035(3) 0.020(2) 0.003(3) 0.0046(18) 0.002(3) C13 0.021(2) 0.030(3) 0.017(2) -0.004(2) -0.0017(19) 0.000(2) C1 0.023(2) 0.028(3) 0.022(2) 0.001(2) 0.0006(19) -0.003(2) C15 0.022(2) 0.032(3) 0.023(2) 0.000(2) 0.0037(19) 0.000(2) C5 0.035(3) 0.029(3) 0.025(2) 0.006(2) 0.005(2) 0.008(2) C3 0.036(3) 0.037(3) 0.020(2) -0.002(2) 0.003(2) 0.010(3) C20 0.027(3) 0.038(4) 0.027(2) 0.003(2) 0.005(2) 0.001(3) C14 0.025(3) 0.028(3) 0.021(2) 0.0027(19) 0.000(2) 0.000(2) C6 0.042(3) 0.031(3) 0.025(3) -0.003(2) 0.007(2) 0.006(2) C12 0.055(4) 0.064(5) 0.029(3) 0.009(3) 0.004(3) 0.023(4) 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' Br Br -0.6763 1.2805 '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' 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 C16 O19 C20 116.6(5) . . ? C4 O11 C12 117.4(5) . . ? O19 C16 C17 115.7(5) . . ? O19 C16 C15 124.7(5) . . ? C15 C16 C17 119.6(5) . . ? C16 C17 H17 120.2 . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17 120.2 . . ? C17 C18 H18 119.3 . . ? C17 C18 C13 121.4(5) . . ? C13 C18 H18 119.3 . . ? Br9 C8 Br10 114.1(3) . . ? C7 C8 Br10 122.6(4) . . ? C7 C8 Br9 123.2(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C3 C2 C1 120.4(5) . . ? C8 C7 C13 120.8(5) . . ? C8 C7 C1 122.1(5) . . ? C1 C7 C13 117.0(4) . . ? O11 C4 C5 124.8(6) . . ? O11 C4 C3 115.6(5) . . ? C5 C4 C3 119.6(5) . . ? C18 C13 C7 121.3(5) . . ? C18 C13 C14 118.7(5) . . ? C14 C13 C7 120.0(5) . . ? C2 C1 C7 120.3(5) . . ? C6 C1 C2 118.9(5) . . ? C6 C1 C7 120.6(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 C16 119.9(5) . . ? C14 C15 H15 120.1 . . ? C4 C5 H5 120.3 . . ? C6 C5 C4 119.5(5) . . ? C6 C5 H5 120.3 . . ? C2 C3 C4 120.2(5) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? O19 C20 H20A 109.5 . . ? O19 C20 H20B 109.5 . . ? O19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C14 H14 119.6 . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C1 C6 C5 121.4(5) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? O11 C12 H12A 109.5 . . ? O11 C12 H12B 109.5 . . ? O11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br10 C8 1.904(5) . ? Br9 C8 1.890(6) . ? O19 C16 1.357(7) . ? O19 C20 1.432(6) . ? O11 C4 1.362(6) . ? O11 C12 1.433(8) . ? C16 C17 1.406(8) . ? C16 C15 1.393(8) . ? C17 H17 0.9300 . ? C17 C18 1.382(8) . ? C18 H18 0.9300 . ? C18 C13 1.388(8) . ? C8 C7 1.322(7) . ? C2 H2 0.9300 . ? C2 C1 1.395(8) . ? C2 C3 1.386(7) . ? C7 C13 1.495(8) . ? C7 C1 1.492(7) . ? C4 C5 1.391(8) . ? C4 C3 1.397(9) . ? C13 C14 1.399(7) . ? C1 C6 1.381(8) . ? C15 H15 0.9300 . ? C15 C14 1.389(7) . ? C5 H5 0.9300 . ? C5 C6 1.390(8) . ? C3 H3 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C14 H14 0.9300 . ? C6 H6 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? 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 Br10 C8 C7 C13 -4.0(8) . . . . ? Br10 C8 C7 C1 176.7(4) . . . . ? Br9 C8 C7 C13 178.6(4) . . . . ? Br9 C8 C7 C1 -0.7(8) . . . . ? O19 C16 C17 C18 -178.8(5) . . . . ? O19 C16 C15 C14 179.3(5) . . . . ? O11 C4 C5 C6 178.4(6) . . . . ? O11 C4 C3 C2 -178.0(5) . . . . ? C16 C17 C18 C13 0.3(8) . . . . ? C16 C15 C14 C13 -1.4(8) . . . . ? C17 C16 C15 C14 -0.2(7) . . . . ? C17 C18 C13 C7 179.8(5) . . . . ? C17 C18 C13 C14 -1.8(8) . . . . ? C18 C13 C14 C15 2.4(7) . . . . ? C8 C7 C13 C18 -72.1(7) . . . . ? C8 C7 C13 C14 109.5(6) . . . . ? C8 C7 C1 C2 96.7(7) . . . . ? C8 C7 C1 C6 -87.5(7) . . . . ? C2 C1 C6 C5 0.2(9) . . . . ? C7 C13 C14 C15 -179.2(5) . . . . ? C7 C1 C6 C5 -175.6(5) . . . . ? C4 C5 C6 C1 0.1(9) . . . . ? C13 C7 C1 C2 -82.6(6) . . . . ? C13 C7 C1 C6 93.3(6) . . . . ? C1 C2 C3 C4 -0.9(9) . . . . ? C1 C7 C13 C18 107.1(6) . . . . ? C1 C7 C13 C14 -71.3(6) . . . . ? C15 C16 C17 C18 0.8(8) . . . . ? C5 C4 C3 C2 1.3(9) . . . . ? C3 C2 C1 C7 176.0(5) . . . . ? C3 C2 C1 C6 0.1(9) . . . . ? C3 C4 C5 C6 -0.9(9) . . . . ? C20 O19 C16 C17 171.4(4) . . . . ? C20 O19 C16 C15 -8.1(7) . . . . ? C12 O11 C4 C5 1.4(9) . . . . ? C12 O11 C4 C3 -179.3(6) . . . . ?