#------------------------------------------------------------------------------ #$Date: 2017-09-12 07:03:26 +0300 (Tue, 12 Sep 2017) $ #$Revision: 200734 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/63/1546374.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_1546374 loop_ _publ_author_name 'Kotani, Shunsuke' 'Kai, Kosuke' 'Sugiura, Masaharu' 'Nakajima, Makoto' _publ_section_title ; Sequential Catalysis of Phosphine Oxide for Stereoselective Synthesis of Stereopentads. ; _journal_issue 13 _journal_name_full 'Organic letters' _journal_page_first 3672 _journal_page_last 3675 _journal_paper_doi 10.1021/acs.orglett.7b01719 _journal_volume 19 _journal_year 2017 _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' _chemical_formula_moiety 'C31 H28 Br2 O3' _chemical_formula_sum 'C31 H28 Br2 O3' _chemical_formula_weight 608.37 _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' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 93.226(2) _cell_angle_gamma 90.0000 _cell_formula_units_Z 2 _cell_length_a 10.1299(10) _cell_length_b 8.6369(8) _cell_length_c 15.8434(15) _cell_measurement_reflns_used 11754 _cell_measurement_temperature 296 _cell_measurement_theta_max 27.43 _cell_measurement_theta_min 3.10 _cell_volume 1384.0(2) _computing_cell_refinement 'RAPID AUTO' _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_data_reduction 'RAPID AUTO' _computing_molecular_graphics 'CrystalStructure 4.2' _computing_publication_material 'CrystalStructure 4.2 (Rigaku, 2015)' _computing_structure_refinement 'SHELXL Version 2016/6 (Sheldrick, 2008)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 296 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 22216 _diffrn_reflns_point_group_measured_fraction_full 0.916 _diffrn_reflns_point_group_measured_fraction_max 0.902 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 3.102 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.967 _exptl_absorpt_correction_T_max 0.169 _exptl_absorpt_correction_T_min 0.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 616.00 _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.600 _refine_diff_density_max 0.48 _refine_diff_density_min -0.36 _refine_ls_abs_structure_details ; Flack x determined using 1043 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.027(8) _refine_ls_extinction_coef 0.025(5) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 326 _refine_ls_number_reflns 5734 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0593 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1029P)^2^+0.2384P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1763 _refine_ls_wR_factor_ref 0.2072 _reflns_Friedel_coverage 0.694 _reflns_Friedel_fraction_full 0.821 _reflns_Friedel_fraction_max 0.792 _reflns_number_gt 3299 _reflns_number_total 5734 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file ol7b01719_si_002.cif _cod_data_source_block 2,4-dibenzyl-1,5-bis(4-bromophenyl)-3-pentanone_(major) _cod_depositor_comments 'Adding full bibliography for 1546374.cif.' _cod_database_code 1546374 _shelx_res_file ; TITL 2,4-dibenzyl-1,5-bis(4-bromophenyl)-3-pentanone (major) shelxl.res created by SHELXL-2016/6 at 11:27:51 on 16-Feb-2017 CELL 0.71075 10.12989 8.63690 15.84340 90.00000 93.22590 90.00000 ZERR 2 0.00100 0.00080 0.00150 0.00000 0.00220 0.00000 LATT -1 SYMM -X, .50+Y, -Z SFAC C H BR O UNIT 62 56 4 6 L.S. 20 FMAP 2 PLAN 50 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 23.0 ACTA SIZE 0.700 0.600 0.600 WGHT 0.102900 0.238400 EXTI 0.025062 FVAR 0.94632 BR1 3 0.608068 0.556542 0.323681 11.00000 0.07972 0.15411 = 0.07557 0.03599 -0.00532 0.01607 BR2 3 1.629351 -0.043932 0.940064 11.00000 0.08525 0.18052 = 0.10008 0.05198 0.01157 0.03219 O1 4 0.620993 0.451578 0.748090 11.00000 0.05570 0.11160 = 0.08174 0.01609 0.01155 0.01309 AFIX 83 H1 2 0.634422 0.425010 0.797517 11.00000 -1.20000 AFIX 0 O2 4 0.990898 0.173189 0.976471 11.00000 0.09209 0.10536 = 0.05303 0.01454 0.01226 0.01851 AFIX 83 H2A 2 0.916090 0.209549 0.971471 11.00000 -1.20000 AFIX 0 O33 4 0.801892 0.308981 0.863750 11.00000 0.09237 0.09347 = 0.05524 0.00869 0.01590 0.02291 C2 1 0.845667 0.368481 0.721487 11.00000 0.04420 0.04918 = 0.05115 0.00531 -0.00199 -0.00147 AFIX 13 H2 2 0.895217 0.313369 0.679418 11.00000 -1.20000 AFIX 0 C3 1 1.041272 0.560146 0.740334 11.00000 0.05372 0.05067 = 0.05963 0.00826 -0.00053 0.00530 C4 1 0.630722 0.493366 0.437860 11.00000 0.05185 0.08173 = 0.07414 0.00771 -0.00410 0.00121 C5 1 0.672230 0.404824 0.606850 11.00000 0.04769 0.05623 = 0.06590 0.00797 -0.01049 -0.00545 C6 1 0.892950 0.538661 0.724604 11.00000 0.05642 0.05526 = 0.07272 0.00599 -0.00295 -0.00229 AFIX 23 H6A 2 0.865850 0.587959 0.671410 11.00000 -1.20000 H6B 2 0.848573 0.591795 0.768909 11.00000 -1.20000 AFIX 0 C7 1 1.004990 0.202456 0.823061 11.00000 0.06381 0.05229 = 0.04456 -0.00257 0.00376 0.00616 AFIX 13 H7 2 1.067234 0.236476 0.781674 11.00000 -1.20000 AFIX 0 C8 1 0.920559 -0.015373 0.721970 11.00000 0.05928 0.05096 = 0.06351 -0.00366 0.00218 0.00617 C9 1 1.204050 0.165842 0.920024 11.00000 0.07276 0.06511 = 0.03852 0.00356 -0.00924 -0.00963 C10 1 0.696872 0.356538 0.695242 11.00000 0.05233 0.05640 = 0.05903 -0.00047 0.00223 -0.00482 AFIX 13 H10 2 0.668719 0.248671 0.700961 11.00000 -1.20000 AFIX 0 C11 1 0.722481 0.319018 0.541434 11.00000 0.06789 0.05566 = 0.06032 0.00662 0.00217 0.00028 AFIX 43 H11 2 0.769560 0.228997 0.554711 11.00000 -1.20000 AFIX 0 C12 1 1.235147 0.045162 0.975571 11.00000 0.08512 0.08478 = 0.05392 0.03212 -0.00334 -0.00049 AFIX 43 H12 2 1.170562 0.005540 1.009015 11.00000 -1.20000 AFIX 0 C13 1 1.125945 0.512888 0.682910 11.00000 0.08189 0.08817 = 0.06201 0.00864 0.01023 -0.00331 AFIX 43 H13 2 1.092875 0.464920 0.633593 11.00000 -1.20000 AFIX 0 C14 1 1.088951 0.632835 0.815147 11.00000 0.07471 0.05229 = 0.06968 -0.00341 -0.00174 0.00107 AFIX 43 H14 2 1.032607 0.664573 0.856162 11.00000 -1.20000 AFIX 0 C15 1 0.877406 0.294598 0.807325 11.00000 0.06410 0.04791 = 0.05240 -0.00231 0.00838 0.00452 C16 1 1.068364 0.232384 0.910532 11.00000 0.07457 0.06773 = 0.04019 0.00390 -0.00748 0.00504 AFIX 13 H16 2 1.075799 0.344731 0.918052 11.00000 -1.20000 AFIX 0 C17 1 1.458751 0.036645 0.933139 11.00000 0.06721 0.10840 = 0.04884 0.00905 0.00240 0.00064 C18 1 1.303030 0.225244 0.873849 11.00000 0.07952 0.07154 = 0.04809 0.01002 -0.00710 -0.01050 AFIX 43 H18 2 1.283820 0.308257 0.837840 11.00000 -1.20000 AFIX 0 C19 1 0.977433 0.027415 0.807908 11.00000 0.07400 0.05805 = 0.06172 0.00117 -0.01394 -0.00185 AFIX 23 H19A 2 1.059771 -0.028577 0.818216 11.00000 -1.20000 H19B 2 0.917101 -0.007644 0.849325 11.00000 -1.20000 AFIX 0 C20 1 0.596600 0.535428 0.584500 11.00000 0.05833 0.07820 = 0.06871 0.00538 0.00327 0.01096 AFIX 43 H20 2 0.558376 0.593014 0.626308 11.00000 -1.20000 AFIX 0 C21 1 0.790663 -0.052832 0.706217 11.00000 0.07803 0.06010 = 0.08219 -0.00333 -0.00522 -0.00955 AFIX 43 H21 2 0.733354 -0.048536 0.750000 11.00000 -1.20000 AFIX 0 C22 1 0.704989 0.362715 0.457147 11.00000 0.06396 0.07925 = 0.06854 -0.00559 -0.00094 0.00685 AFIX 43 H22 2 0.742307 0.305492 0.414843 11.00000 -1.20000 AFIX 0 C23 1 0.742299 -0.097288 0.626014 11.00000 0.06348 0.07049 = 0.09223 -0.01054 -0.00725 0.00114 AFIX 43 H23 2 0.654114 -0.126156 0.617459 11.00000 -1.20000 AFIX 0 C24 1 0.578055 0.579881 0.500648 11.00000 0.06013 0.07314 = 0.08427 0.02151 -0.00908 0.01626 AFIX 43 H24 2 0.529723 0.668719 0.486731 11.00000 -1.20000 AFIX 0 C25 1 1.429419 0.166674 0.878826 11.00000 0.08208 0.08972 = 0.04092 0.00950 -0.00261 -0.01850 AFIX 43 H25 2 1.494809 0.210537 0.847542 11.00000 -1.20000 AFIX 0 C26 1 1.000320 -0.017732 0.654344 11.00000 0.05775 0.11724 = 0.07960 -0.03102 0.01212 0.00142 AFIX 43 H26 2 1.088936 0.009097 0.663154 11.00000 -1.20000 AFIX 0 C27 1 0.820799 -0.099082 0.561107 11.00000 0.08846 0.09486 = 0.06542 -0.01813 -0.01271 0.00584 AFIX 43 H27 2 0.787301 -0.127282 0.507442 11.00000 -1.20000 AFIX 0 C28 1 1.360218 -0.016108 0.981555 11.00000 0.07403 0.09901 = 0.06784 0.02964 -0.00799 0.00215 AFIX 43 H28 2 1.378781 -0.096064 1.019711 11.00000 -1.20000 AFIX 0 C29 1 0.953534 -0.058260 0.574545 11.00000 0.08672 0.14208 = 0.06129 -0.02720 0.00354 0.00182 AFIX 43 H29 2 1.009498 -0.058540 0.529983 11.00000 -1.20000 AFIX 0 C30 1 1.263098 0.534528 0.695945 11.00000 0.06174 0.08404 = 0.11201 0.01615 0.02453 -0.00655 AFIX 43 H30 2 1.320378 0.498039 0.656619 11.00000 -1.20000 AFIX 0 C31 1 1.310336 0.608131 0.765486 11.00000 0.06345 0.08353 = 0.14739 0.03760 -0.00527 -0.01601 AFIX 43 H31 2 1.400562 0.627173 0.773260 11.00000 -1.20000 AFIX 0 C32 1 1.227374 0.655298 0.824883 11.00000 0.08829 0.08011 = 0.10567 0.00028 -0.03014 -0.01010 AFIX 43 H32 2 1.262661 0.703861 0.873453 11.00000 -1.20000 AFIX 0 HKLF 4 REM 2,4-dibenzyl-1,5-bis(4-bromophenyl)-3-pentanone (major) REM R1 = 0.0593 for 3299 Fo > 4sig(Fo) and 0.1028 for all 5734 data REM 326 parameters refined using 1 restraints END WGHT 0.1029 0.2384 REM Instructions for potential hydrogen bonds HTAB O1 O33 HTAB O2 O33 REM Highest difference peak 0.480, deepest hole -0.356, 1-sigma level 0.095 Q1 1 0.5403 0.4684 0.3240 11.00000 0.05 0.48 Q2 1 0.4342 0.5601 0.3178 11.00000 0.05 0.47 Q3 1 1.2067 0.0597 0.6728 11.00000 0.05 0.46 Q4 1 1.7874 -0.0393 0.9378 11.00000 0.05 0.45 Q5 1 0.7353 0.5072 0.3065 11.00000 0.05 0.44 Q6 1 1.5377 -0.0911 0.8765 11.00000 0.05 0.43 Q7 1 1.5234 0.0287 0.9673 11.00000 0.05 0.43 Q8 1 1.5406 0.0669 0.9658 11.00000 0.05 0.43 Q9 1 1.5838 -0.1373 0.9156 11.00000 0.05 0.41 Q10 1 0.5116 0.5372 0.2621 11.00000 0.05 0.40 Q11 1 1.7171 0.0579 0.9371 11.00000 0.05 0.39 Q12 1 0.6168 0.4564 0.3807 11.00000 0.05 0.38 Q13 1 1.4521 -0.0721 0.9397 11.00000 0.05 0.38 Q14 1 1.6067 0.0414 0.9288 11.00000 0.05 0.38 Q15 1 1.7375 0.0222 1.0034 11.00000 0.05 0.37 Q16 1 0.8370 0.4538 0.7321 11.00000 0.05 0.37 Q17 1 0.7016 0.5801 0.3860 11.00000 0.05 0.37 Q18 1 0.6219 0.6319 0.3753 11.00000 0.05 0.34 Q19 1 1.2437 0.4772 0.6061 11.00000 0.05 0.30 Q20 1 1.7192 0.1270 0.9605 11.00000 0.05 0.29 Q21 1 1.6059 -0.0214 0.9838 11.00000 0.05 0.28 Q22 1 1.2625 0.5556 0.5819 11.00000 0.05 0.27 Q23 1 0.8850 -0.0309 0.5626 11.00000 0.05 0.27 Q24 1 0.8047 0.3782 0.7389 11.00000 0.05 0.27 Q25 1 0.6604 0.5483 0.4867 11.00000 0.05 0.27 Q26 1 0.9219 0.0592 0.9652 11.00000 0.05 0.27 Q27 1 0.8943 -0.0629 0.5718 11.00000 0.05 0.27 Q28 1 1.5689 -0.1555 0.9944 11.00000 0.05 0.27 Q29 1 1.2228 0.5500 0.7405 11.00000 0.05 0.26 Q30 1 1.1749 0.5510 0.7033 11.00000 0.05 0.26 Q31 1 0.6455 0.5265 0.4229 11.00000 0.05 0.25 Q32 1 0.6227 0.5667 0.4389 11.00000 0.05 0.25 Q33 1 0.9683 -0.0474 0.6557 11.00000 0.05 0.25 Q34 1 1.0322 0.3966 0.7368 11.00000 0.05 0.25 Q35 1 1.0029 0.0225 0.9326 11.00000 0.05 0.25 Q36 1 0.8838 0.0939 0.9193 11.00000 0.05 0.25 Q37 1 1.2263 0.1042 0.9384 11.00000 0.05 0.24 Q38 1 0.6616 0.5286 0.7985 11.00000 0.05 0.24 Q39 1 1.3117 -0.0142 0.9669 11.00000 0.05 0.24 Q40 1 0.6530 0.6266 0.7554 11.00000 0.05 0.24 Q41 1 1.6864 0.0414 0.8804 11.00000 0.05 0.24 Q42 1 0.5425 0.4446 0.3808 11.00000 0.05 0.24 Q43 1 0.9706 0.0881 1.0417 11.00000 0.05 0.24 Q44 1 1.4463 0.5538 0.7857 11.00000 0.05 0.24 Q45 1 1.0825 0.0391 0.9404 11.00000 0.05 0.24 Q46 1 0.9319 -0.0743 0.6219 11.00000 0.05 0.23 Q47 1 1.1289 0.0374 1.0104 11.00000 0.05 0.23 Q48 1 1.2242 0.4172 0.7547 11.00000 0.05 0.23 Q49 1 1.4135 0.5194 0.7676 11.00000 0.05 0.23 Q50 1 0.6416 0.4299 0.5964 11.00000 0.05 0.22 ; _shelx_res_checksum 31773 _shelx_hkl_file ; 0 0 3 5668.85 426.57 0 0 3 5392.72 392.81 0 0 -3 5543.83 406.64 0 0 -3 5561.58 398.12 0 0 4 105.46 8.60 0 0 4 106.87 4.43 0 0 -4 99.56 7.39 0 0 -4 103.33 5.26 0 0 5 2944.13 165.33 0 0 5 3124.68 191.92 0 0 -5 3151.13 169.53 0 0 -5 2905.70 166.12 0 0 6 164.99 8.87 0 0 6 170.54 7.73 0 0 -6 172.79 12.93 0 0 -6 167.50 9.44 0 0 7 27.49 9.68 0 0 7 27.04 4.47 0 0 -7 29.57 4.77 0 0 -7 33.66 10.33 0 0 8 4339.43 338.24 0 0 8 4528.23 342.08 0 0 -8 4792.11 354.12 0 0 -8 4489.39 355.03 0 0 9 10.31 5.27 0 0 9 11.34 6.05 0 0 -9 6.56 6.73 0 0 -9 11.32 5.13 0 0 10 81.27 16.67 0 0 10 84.04 10.98 0 0 -10 94.54 21.77 0 0 -10 86.69 9.48 0 0 11 243.83 21.09 0 0 11 256.27 18.52 0 0 -11 266.02 25.10 0 0 -11 262.95 30.27 0 0 12 112.86 21.52 0 0 12 83.61 25.26 0 0 -12 77.13 11.61 0 0 -12 111.14 17.18 0 0 13 1.95 7.02 0 0 13 -3.18 8.13 0 0 -13 -0.15 12.66 0 0 -13 2.28 17.62 0 0 14 61.39 15.87 0 0 14 89.52 25.06 0 0 -14 87.98 13.67 0 0 -14 65.98 19.22 0 0 15 222.27 25.04 0 0 15 183.93 47.56 0 0 -15 231.35 40.41 0 0 -15 214.48 33.52 0 0 16 215.33 30.37 0 0 16 243.30 47.68 0 0 -16 238.07 37.07 0 0 -16 232.52 25.85 0 0 17 42.18 16.02 0 0 17 27.68 16.69 0 0 -17 42.79 24.56 0 0 -17 64.30 21.11 0 0 18 -0.45 22.53 0 0 18 -2.41 13.44 0 0 -18 -9.14 11.10 0 0 -18 -22.73 31.76 0 0 19 28.47 16.26 0 0 19 9.25 15.23 0 0 -19 18.03 23.13 0 0 -19 19.87 22.40 0 0 20 30.02 33.23 0 0 20 35.72 37.45 0 0 -20 24.16 29.47 0 0 -20 59.70 16.68 0 1 2 994.77 30.79 0 1 2 1027.75 31.80 0 1 -2 1060.49 32.57 0 1 -2 1125.69 29.65 0 -1 2 1176.54 33.70 0 -1 -2 1062.75 28.52 0 -1 2 1100.33 34.63 0 -1 -2 1096.56 34.67 0 1 312158.72 1545.11 0 1 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75.71 7.45 0 7 -5 93.50 19.72 0 7 -5 97.83 29.20 0 7 6 12.22 10.07 0 7 6 13.25 8.80 0 7 6 -0.04 7.38 0 7 6 10.60 6.10 0 7 -6 9.98 10.02 0 7 -6 0.70 2.24 0 7 -6 7.50 3.60 0 -7 6 6.44 11.89 0 7 -7 60.46 5.98 0 7 7 83.11 8.88 0 7 7 64.33 14.77 0 7 7 74.34 9.77 0 7 -7 57.55 17.61 0 -7 7 69.70 20.25 0 -7 7 72.36 6.27 0 7 8 54.55 13.32 0 7 8 56.64 14.61 0 7 8 67.21 14.09 0 7 8 56.80 8.05 0 7 -8 43.17 5.49 0 7 -8 51.46 17.17 0 -7 8 57.88 5.66 0 -7 8 66.94 19.84 0 7 9 62.55 13.55 0 7 9 79.79 31.98 0 7 9 68.51 16.60 0 7 9 68.14 8.37 0 7 -9 65.05 18.75 0 -7 9 81.71 41.42 0 7 10 -8.60 19.86 0 7 -10 11.23 12.82 0 7 10 -7.37 12.05 0 7 10 -0.01 7.66 0 7 10 4.66 4.55 0 7 -10 3.39 4.06 0 -7 10 5.31 4.04 0 -7 10 -3.95 27.46 0 7 11 -0.00 7.31 0 7 11 7.97 12.12 0 7 -11 32.45 15.14 0 7 11 24.03 13.85 0 7 -11 6.38 4.90 0 7 11 9.74 7.68 0 -7 11 0.82 18.49 0 -7 11 7.93 4.66 0 7 12 23.58 23.30 0 7 12 1.91 6.31 0 7 -12 7.48 5.51 0 7 12 2.14 6.78 0 7 12 1.04 14.47 0 7 -12 24.12 27.56 0 -7 12 0.59 19.58 0 -7 12 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5 25.17 14.33 0 8 -5 23.22 4.20 0 8 -5 30.02 15.94 0 8 -5 22.91 4.19 0 8 -5 32.31 13.48 0 8 6 0.08 13.42 0 8 6 8.43 8.69 0 8 6 -0.08 6.04 0 8 6 4.23 6.88 0 8 -6 22.76 25.52 0 8 -6 1.65 2.99 0 8 -6 1.51 2.75 0 8 -6 -5.38 20.03 0 8 7 9.84 5.61 0 8 7 10.37 11.55 0 8 7 4.85 8.49 0 8 7 3.49 16.44 0 8 -7 -1.73 11.99 0 8 -7 1.81 2.34 0 8 -7 0.54 1.29 0 8 -7 14.75 14.85 0 8 8 3.86 9.41 0 8 8 9.35 10.59 0 8 8 -0.02 10.47 0 8 8 4.20 9.45 0 8 -8 -0.23 23.39 0 8 -8 1.40 2.10 0 8 -8 2.08 1.97 0 8 -8 1.55 15.87 0 8 9 -11.76 20.66 0 8 9 3.48 12.39 0 8 9 -0.00 10.79 0 8 9 20.24 9.80 0 8 -9 6.21 14.31 0 -8 9 15.15 17.04 0 8 10 31.09 13.08 0 8 10 19.83 5.76 0 8 10 0.02 9.90 0 8 10 5.03 26.07 0 8 -10 44.25 30.13 0 -8 10 33.53 20.43 0 8 11 0.01 7.29 0 8 11 14.61 13.69 0 8 11 -1.77 22.02 0 8 -11 18.42 16.14 0 8 11 1.45 4.52 0 -8 11 27.55 18.85 0 8 12 -30.56 13.35 0 8 12 21.96 14.65 0 8 -12 44.05 29.99 0 -8 12 -5.73 20.19 0 8 13 -3.33 16.56 0 8 13 -1.11 15.18 0 8 -13 -19.74 18.62 0 -8 13 0.63 22.63 0 8 14 19.86 19.84 0 8 14 25.12 32.09 0 8 -14 8.98 39.55 0 -8 14 0.22 26.92 0 9 0 -11.85 9.30 0 9 0 2.02 3.91 0 9 0 -2.87 7.66 0 9 0 -3.98 10.81 0 9 1 7.29 5.70 0 9 1 7.02 9.90 0 9 1 12.23 8.92 0 9 1 10.05 11.21 0 9 -1 11.18 7.19 0 9 -1 8.73 10.84 0 9 -1 11.15 3.91 0 9 -1 -0.97 12.79 0 9 2 -4.58 9.68 0 9 2 3.52 10.13 0 9 2 -5.90 8.86 0 9 2 -6.00 14.51 0 9 -2 -0.40 3.04 0 9 -2 3.33 5.01 0 9 -2 -8.81 10.10 0 9 -2 8.04 21.62 0 9 3 -0.58 6.39 0 9 3 -0.85 5.59 0 9 3 -0.06 9.30 0 9 3 4.75 7.69 0 9 -3 1.61 4.26 0 9 -3 -7.22 12.92 0 9 -3 4.94 19.50 0 9 -3 0.71 4.27 0 9 4 -1.66 13.18 0 9 4 24.95 10.41 0 9 4 16.47 8.66 0 9 4 0.12 8.51 0 9 -4 23.77 4.29 0 9 -4 13.24 2.42 0 9 -4 25.86 15.14 0 9 -4 21.99 13.35 0 9 5 -1.16 12.79 0 9 5 4.35 7.02 0 9 5 9.40 15.32 0 9 5 0.09 8.15 0 9 -5 5.80 13.77 0 9 -5 -6.93 22.03 0 9 6 7.08 8.33 0 9 6 3.71 8.29 0 9 6 7.23 17.25 0 9 6 -1.58 12.24 0 9 -6 -5.18 29.74 0 9 -6 18.53 13.46 0 9 7 37.17 16.99 0 9 7 14.12 20.24 0 9 7 15.88 14.36 0 9 7 23.76 13.12 0 9 -7 48.79 17.91 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-1 -1.23 33.90 -11 -5 1 1.46 11.04 -11 -5 1 15.22 18.24 11 5 0 20.02 15.34 11 5 0 21.41 21.28 -11 5 0 23.08 15.90 -11 5 0 -1.36 12.39 11 -5 0 10.43 11.47 -11 -5 0 11.80 7.68 -11 -5 0 33.71 20.81 11 -5 0 29.40 21.07 11 5 1 39.03 32.69 11 5 1 6.13 8.32 -11 5 -1 -1.39 14.24 -11 5 -1 5.13 12.35 11 -5 1 -2.96 11.32 -11 -5 -1 -3.31 13.43 -11 -5 -1 -7.06 34.38 11 -5 1 19.32 18.38 11 5 2 -8.56 8.92 11 5 2 -8.21 17.85 -11 5 -2 3.48 13.43 -11 5 -2 -21.37 23.00 11 -5 2 8.20 13.57 -11 -5 -2 16.91 8.37 -11 -5 -2 2.28 19.86 11 -5 2 -10.25 32.87 11 5 3 33.79 23.38 11 5 3 26.31 22.32 -11 5 -3 22.85 31.30 -11 5 -3 38.60 18.97 11 -5 3 41.20 20.31 -11 -5 -3 23.79 20.97 -11 -5 -3 101.38 46.61 11 -5 3 19.20 24.18 11 5 4 -22.70 17.36 11 5 4 -4.57 19.82 -11 5 -4 -2.48 14.03 -11 5 -4 1.71 29.42 11 -5 4 1.38 16.97 -11 -5 -4 3.93 10.25 -11 -5 -4 -20.02 21.39 11 -5 4 -26.71 34.50 11 5 5 8.33 17.99 11 5 5 22.72 12.74 -11 5 -5 -20.63 14.96 -11 5 -5 3.19 20.63 11 -5 5 13.30 40.32 -11 -5 -5 5.07 12.04 -11 -5 -5 26.16 22.98 11 -5 5 43.64 21.18 11 6 -3 -31.91 21.81 -11 6 3 0.28 18.54 -11 -6 3 11.53 22.57 11 -6 -3 -13.71 45.66 11 6 -2 35.94 37.62 -11 6 2 -4.71 16.65 -11 6 2 -4.74 8.44 11 -6 -2 14.81 22.97 11 -6 -2 -7.90 8.02 -11 -6 2 -16.93 20.50 11 6 -1 49.06 21.11 -11 6 1 18.37 30.08 -11 6 1 3.26 10.16 11 -6 -1 34.36 23.52 11 -6 -1 -25.24 16.85 -11 -6 1 14.13 21.21 11 6 0 0.26 7.18 11 6 0 -0.73 38.40 -11 6 0 7.25 16.15 -11 6 0 38.65 11.84 11 -6 0 23.85 11.40 -11 -6 0 2.15 11.66 -11 -6 0 -13.71 23.91 11 -6 0 43.64 23.52 11 6 1 3.72 12.87 11 6 1 -3.75 20.91 -11 6 -1 23.40 14.89 -11 6 -1 -4.36 21.47 11 -6 1 -14.81 11.94 -11 -6 -1 5.07 12.33 -11 -6 -1 37.36 22.06 11 -6 1 6.50 20.46 12 0 -9 -1.56 7.73 12 0 -9 -12.79 15.68 -12 0 9 -6.72 8.49 -12 0 9 7.66 13.26 12 0 -8 -6.63 14.06 12 0 -8 19.38 14.42 -12 0 8 -3.43 8.74 -12 0 8 14.70 22.48 12 0 -7 21.41 17.81 12 0 -7 41.39 17.85 -12 0 7 13.94 18.45 -12 0 7 13.65 15.38 12 0 -6 7.65 10.19 12 0 -6 41.35 16.36 -12 0 6 24.50 20.34 -12 0 6 15.27 13.84 12 0 -5 9.85 9.33 12 0 -5 -8.34 14.29 -12 0 5 3.32 19.01 -12 0 5 1.23 21.34 12 0 -4 22.63 17.93 12 0 -4 -2.79 13.24 -12 0 4 -4.55 18.71 -12 0 4 -1.16 11.67 12 0 -3 -20.31 12.09 12 0 -3 16.50 26.05 -12 0 3 4.64 22.97 -12 0 3 -14.06 20.28 12 0 -2 3.73 12.25 12 0 -2 8.05 25.97 -12 0 2 4.06 23.96 -12 0 2 14.34 11.19 12 0 -1 12.21 21.92 12 0 -1 5.02 13.95 -12 0 1 -4.19 14.28 -12 0 1 8.90 11.08 12 0 0 21.56 13.46 12 0 0 -4.57 15.13 -12 0 0 8.15 15.42 -12 0 0 0.30 20.77 12 0 1 22.15 13.75 12 0 1 26.88 17.11 -12 0 -1 51.35 31.53 -12 0 -1 2.61 12.80 12 0 2 -1.62 12.79 12 0 2 -22.75 28.36 -12 0 -2 -25.67 16.89 -12 0 -2 1.74 11.76 12 0 3 -0.10 12.18 12 0 3 6.63 14.84 -12 0 -3 -37.47 30.47 -12 0 -3 0.66 11.10 12 0 4 -0.42 27.58 12 0 4 25.87 18.57 -12 0 -4 49.06 21.72 -12 0 -4 -1.40 14.31 12 0 5 -1.20 14.03 12 0 5 12.89 30.58 -12 0 -5 0.54 13.00 -12 0 -5 21.68 35.59 12 0 6 -2.10 26.46 12 0 6 -3.05 18.11 -12 0 -6 0.09 13.80 -12 0 -6 -6.73 21.01 12 0 7 -51.97 35.87 12 0 7 -2.80 15.76 -12 0 -7 -2.20 26.57 -12 0 -7 18.44 23.26 12 1 -9 29.22 19.82 12 1 -9 17.97 15.17 -12 1 9 2.36 28.19 -12 1 9 6.78 7.46 12 -1 -9 0.06 11.42 12 -1 -9 31.26 20.25 -12 -1 9 17.43 11.42 12 1 -8 9.00 13.56 -12 1 8 11.63 12.78 -12 1 8 12.30 14.65 12 1 -8 9.96 10.77 -12 -1 8 11.52 11.47 -12 -1 8 -16.41 18.50 12 -1 -8 -0.03 11.90 12 -1 -8 5.92 17.68 12 1 -7 -1.29 10.34 12 1 -7 6.76 12.57 -12 1 7 -28.04 25.71 -12 1 7 8.79 7.99 12 -1 -7 -2.04 16.53 -12 -1 7 2.11 10.23 -12 -1 7 3.27 9.69 12 -1 -7 0.05 12.33 12 1 -6 17.84 13.01 -12 1 6 3.38 9.07 -12 1 6 1.33 13.43 12 1 -6 13.96 12.36 -12 -1 6 9.34 11.79 -12 -1 6 17.99 11.21 12 -1 -6 0.04 8.11 12 -1 -6 17.72 16.65 12 1 -5 9.05 12.70 -12 1 5 33.16 16.96 -12 1 5 14.06 21.82 12 1 -5 -2.26 21.56 -12 -1 5 8.64 11.83 -12 -1 5 -20.81 19.29 12 -1 -5 -0.05 8.38 12 -1 -5 -2.07 28.55 12 1 -4 9.75 12.80 -12 1 4 -0.52 18.93 -12 1 4 6.74 12.37 12 1 -4 15.08 13.01 -12 -1 4 4.35 13.10 -12 -1 4 0.13 9.87 12 -1 -4 14.90 9.18 12 -1 -4 13.29 30.07 12 1 -3 91.70 22.31 12 1 -3 102.00 21.45 -12 1 3 87.92 34.70 12 -1 -3 87.08 26.61 12 -1 -3 82.35 29.04 -12 -1 3 83.35 33.73 -12 -1 3 102.13 39.83 12 1 -2 -12.18 12.31 -12 1 2 -5.10 11.86 -12 1 2 -1.86 20.66 12 1 -2 -3.87 12.50 -12 -1 2 11.47 23.73 -12 -1 2 -0.57 10.84 12 -1 -2 0.92 10.50 12 -1 -2 2.40 14.56 12 1 -1 -7.50 22.16 -12 1 1 -0.02 10.54 -12 1 1 2.46 12.03 12 1 -1 -0.39 11.08 -12 -1 1 11.97 13.41 -12 -1 1 -6.33 10.39 12 -1 -1 6.71 10.78 12 -1 -1 -7.46 14.34 12 1 0 -53.80 23.89 -12 1 0 15.64 13.86 -12 1 0 -0.25 11.77 12 1 0 -32.49 21.53 -12 -1 0 33.02 15.56 -12 -1 0 12.25 20.04 12 -1 0 32.06 21.52 12 -1 0 -50.90 27.55 12 1 1 0.18 12.79 12 1 1 -4.99 13.91 -12 1 -1 -1.43 21.89 -12 1 -1 21.88 27.50 12 -1 1 -7.58 16.34 -12 -1 -1 14.39 10.75 -12 -1 -1 39.39 30.39 12 -1 1 6.98 12.62 12 1 2 -14.13 14.68 -12 1 -2 9.19 16.55 -12 1 -2 3.57 12.91 12 1 2 0.65 23.98 -12 -1 -2 10.57 17.86 -12 -1 -2 1.07 11.45 12 -1 2 23.72 12.39 12 -1 2 23.24 16.99 12 1 3 6.37 14.30 -12 1 -3 -0.19 12.28 12 1 3 0.31 13.49 -12 1 -3 7.09 28.97 12 -1 3 -1.44 21.91 -12 -1 -3 -3.54 20.01 12 -1 3 4.80 16.68 12 1 4 -8.57 28.36 -12 1 -4 20.03 17.82 -12 1 -4 -1.84 23.43 12 1 4 0.20 26.03 -12 -1 -4 -0.55 12.69 -12 -1 -4 17.72 19.67 12 -1 4 3.71 17.80 12 -1 4 0.24 13.45 12 1 5 0.47 15.52 12 1 5 28.76 16.85 -12 1 -5 -3.25 13.79 -12 1 -5 13.61 35.54 12 -1 5 0.03 15.76 -12 -1 -5 30.05 22.16 -12 -1 -5 -2.19 14.10 12 -1 5 15.38 19.16 12 1 6 -3.81 30.13 -12 1 -6 4.97 20.53 -12 1 -6 0.10 13.57 12 1 6 -0.56 27.07 -12 -1 -6 -0.85 25.48 -12 -1 -6 8.34 22.21 12 -1 6 6.59 18.85 12 -1 6 -0.00 15.63 12 1 7 -0.19 15.75 12 1 7 36.76 18.80 -12 1 -7 -0.72 24.71 -12 1 -7 1.50 27.11 12 -1 7 -0.69 17.73 -12 -1 -7 14.93 25.35 -12 -1 -7 0.34 15.80 12 -1 7 -7.24 21.38 12 2 -8 2.26 13.46 12 2 -8 1.41 18.97 -12 2 8 1.92 15.71 12 -2 -8 2.76 18.93 -12 -2 8 1.79 8.31 -12 -2 8 9.36 12.52 12 2 -7 -0.23 23.98 12 2 -7 -0.82 19.13 -12 2 7 -0.19 14.42 -12 2 7 -0.71 11.33 12 -2 -7 -0.08 5.57 12 -2 -7 -32.85 32.56 -12 -2 7 0.91 12.45 12 2 -6 -2.19 14.88 12 2 -6 19.07 11.07 -12 2 6 -1.30 14.94 -12 2 6 15.70 13.84 12 -2 -6 75.47 33.95 -12 -2 6 4.34 8.24 -12 -2 6 -1.77 12.27 12 -2 -6 0.76 6.51 12 2 -5 -4.73 13.58 12 2 -5 -3.57 10.34 -12 2 5 0.66 13.39 -12 2 5 3.55 7.69 12 -2 -5 15.78 16.25 -12 -2 5 -3.32 8.15 -12 -2 5 -3.51 12.29 12 -2 -5 0.26 6.57 12 2 -4 48.90 29.21 12 2 -4 19.37 12.18 -12 2 4 -1.73 28.93 -12 2 4 19.70 10.90 12 -2 -4 18.47 19.93 -12 -2 4 11.11 17.94 -12 -2 4 23.37 15.65 12 -2 -4 -1.56 15.58 12 2 -3 36.63 18.37 12 2 -3 22.55 13.75 -12 2 3 -0.86 16.82 -12 2 3 41.93 13.39 12 -2 -3 31.88 21.02 -12 -2 3 34.79 12.08 -12 -2 3 43.95 18.31 12 -2 -3 20.76 18.62 12 2 -2 11.62 23.41 12 2 -2 1.13 11.14 -12 2 2 1.03 13.32 -12 2 2 8.13 11.08 12 -2 -2 -11.90 16.06 -12 -2 2 15.08 17.14 -12 -2 2 -8.57 26.22 12 -2 -2 22.47 29.61 12 2 -1 37.61 16.23 12 2 -1 11.03 14.31 -12 2 1 -0.99 28.62 -12 2 1 30.31 14.68 12 -2 -1 18.74 12.98 -12 -2 1 17.72 12.33 -12 -2 1 40.01 18.37 12 -2 -1 42.99 20.14 12 2 0 -0.32 25.62 12 2 0 19.64 13.12 -12 2 0 -0.05 13.73 -12 2 0 17.15 14.28 12 -2 0 12.19 12.43 -12 -2 0 5.64 17.37 -12 -2 0 14.50 11.35 12 -2 0 -6.28 18.43 12 2 1 -0.01 15.26 12 2 1 25.32 25.77 -12 2 -1 1.22 14.90 -12 2 -1 28.02 29.09 12 -2 1 7.65 25.04 -12 -2 -1 75.84 34.47 -12 -2 -1 46.13 22.42 12 -2 1 15.03 19.99 12 2 2 0.26 14.49 12 2 2 3.68 24.22 -12 2 -2 0.94 24.03 -12 2 -2 25.24 15.38 12 -2 2 -16.65 13.50 -12 -2 -2 -9.14 18.68 -12 -2 -2 10.04 11.82 12 -2 2 24.11 18.16 12 2 3 -0.55 14.34 12 2 3 8.43 14.29 -12 2 -3 -2.21 13.41 -12 2 -3 9.96 29.11 12 -2 3 -12.26 15.00 -12 -2 -3 5.71 36.39 -12 -2 -3 -21.42 12.60 12 -2 3 -5.65 18.63 12 2 4 17.91 16.68 12 2 4 0.12 17.29 -12 2 -4 0.33 15.31 -12 2 -4 48.52 20.69 12 -2 4 -10.72 30.74 -12 -2 -4 36.21 23.72 -12 -2 -4 45.61 27.32 12 -2 4 36.89 39.11 12 2 5 -0.52 27.06 12 2 5 0.73 15.14 -12 2 -5 3.18 23.85 -12 2 -5 1.53 19.02 12 -2 5 -17.56 15.80 -12 -2 -5 4.39 21.16 -12 -2 -5 13.12 13.11 12 -2 5 -37.93 19.29 12 2 6 0.37 14.48 12 2 6 -5.29 15.75 -12 2 -6 2.05 13.06 -12 2 -6 0.56 37.20 12 -2 6 0.17 16.50 -12 -2 -6 -13.61 41.56 -12 -2 -6 9.67 13.77 12 -2 6 -18.81 36.40 12 3 -7 -29.64 31.95 12 3 -7 0.69 9.28 -12 3 7 -0.69 31.35 12 -3 -7 1.27 23.18 -12 -3 7 -9.73 7.05 -12 -3 7 -26.88 27.66 12 3 -6 -20.32 17.10 12 3 -6 -0.97 16.35 -12 3 6 2.22 15.85 -12 3 6 4.73 6.57 12 -3 -6 0.10 5.72 -12 -3 6 5.93 6.84 -12 -3 6 16.76 26.50 12 -3 -6 24.92 20.29 12 3 -5 -16.81 16.92 12 3 -5 -0.53 15.88 -12 3 5 -1.73 27.06 -12 3 5 21.38 12.60 12 -3 -5 0.15 10.83 -12 -3 5 -14.49 11.99 -12 -3 5 -0.40 13.50 12 -3 -5 -4.76 19.09 12 3 -4 -19.51 26.93 12 3 -4 -0.60 9.17 -12 3 4 0.93 15.15 -12 3 4 -7.60 8.75 12 -3 -4 1.39 12.61 -12 -3 4 -7.44 14.91 -12 -3 4 -2.90 7.35 12 -3 -4 -5.25 35.28 12 3 -3 3.67 15.51 12 3 -3 -3.69 9.87 -12 3 3 -0.87 25.95 -12 3 3 -0.64 9.53 12 -3 -3 0.35 14.40 -12 -3 3 -8.58 15.62 -12 -3 3 -25.12 13.79 12 -3 -3 -2.80 19.73 12 3 -2 4.90 28.06 12 3 -2 7.34 10.12 -12 3 2 -1.43 13.88 -12 3 2 10.41 10.35 12 -3 -2 7.00 8.75 -12 -3 2 -33.53 28.78 -12 -3 2 -4.35 7.90 12 -3 -2 4.77 18.13 12 3 -1 0.20 15.20 12 3 -1 3.38 10.59 -12 3 1 0.83 13.89 -12 3 1 -9.23 11.69 12 -3 -1 1.07 9.62 -12 -3 1 -4.03 16.63 -12 -3 1 -11.05 8.30 12 -3 -1 4.21 17.89 12 3 0 -13.95 27.50 12 3 0 11.72 10.61 -12 3 0 0.78 23.90 -12 3 0 -19.73 21.21 12 -3 0 58.55 32.81 12 -3 0 -7.14 10.65 -12 -3 0 17.34 16.83 -12 -3 0 -1.40 15.84 12 3 1 -1.78 14.81 12 3 1 12.89 10.92 -12 3 -1 -1.87 12.86 -12 3 -1 -13.06 12.76 12 -3 1 4.80 17.75 12 -3 1 -12.29 11.95 -12 -3 -1 -2.88 16.96 -12 -3 -1 12.36 9.86 12 3 2 -16.69 22.06 12 3 2 0.33 15.69 -12 3 -2 0.81 13.98 -12 3 -2 17.58 15.38 12 -3 2 11.21 19.31 12 -3 2 27.36 24.87 -12 -3 -2 5.20 19.33 -12 -3 -2 -7.29 20.01 12 3 3 12.47 26.69 12 3 3 0.81 17.76 -12 3 -3 0.60 28.39 -12 3 -3 40.22 19.03 12 -3 3 9.89 16.76 -12 -3 -3 18.79 22.90 -12 -3 -3 15.02 13.48 12 -3 3 35.75 22.41 12 3 4 -2.86 13.68 12 3 4 -0.28 28.22 -12 3 -4 -0.20 13.62 -12 3 -4 4.50 17.94 12 -3 4 19.86 20.40 12 -3 4 4.30 15.16 -12 -3 -4 4.40 22.79 -12 -3 -4 5.84 12.89 12 3 5 0.27 15.89 12 3 5 -10.49 14.68 -12 3 -5 2.31 13.35 -12 3 -5 7.25 18.87 12 -3 5 12.07 21.22 12 -3 5 12.07 16.69 -12 -3 -5 31.55 23.45 -12 -3 -5 -32.87 12.88 12 4 -5 38.59 30.28 12 4 -5 -0.24 7.42 -12 4 5 0.65 16.48 12 -4 -5 2.68 22.32 -12 -4 5 -0.37 10.04 -12 -4 5 19.92 29.65 12 4 -4 16.30 19.00 12 4 -4 -0.26 14.60 -12 4 4 0.18 16.68 -12 4 4 5.87 13.98 12 -4 -4 1.05 6.95 -12 -4 4 -7.44 16.31 -12 -4 4 9.26 6.39 12 -4 -4 25.29 22.93 12 4 -3 6.46 18.09 12 4 -3 0.71 14.22 -12 4 3 0.46 15.68 -12 4 3 7.15 15.15 12 -4 -3 0.69 21.74 12 -4 -3 -1.37 7.52 -12 -4 3 -12.33 17.18 -12 -4 3 -14.60 11.41 12 4 -2 -8.64 31.57 12 4 -2 0.53 8.78 -12 4 2 -1.79 15.17 -12 4 2 -1.13 17.39 12 -4 -2 7.60 8.63 -12 -4 2 -61.74 31.71 -12 -4 2 10.14 7.12 12 -4 -2 -14.82 39.57 12 4 -1 19.59 19.44 12 4 -1 0.27 10.31 -12 4 1 -0.29 29.29 -12 4 1 23.79 20.80 12 -4 -1 5.02 10.43 -12 -4 1 46.01 19.71 -12 -4 1 12.28 14.74 12 -4 -1 25.31 22.68 12 4 0 32.14 31.60 12 4 0 -1.56 10.22 -12 4 0 1.04 15.28 -12 4 0 15.77 21.63 12 -4 0 12.35 10.99 -12 -4 0 9.70 20.07 -12 -4 0 5.15 8.42 12 -4 0 5.45 21.14 12 4 1 2.65 10.25 12 4 1 15.76 16.46 -12 4 -1 2.03 13.63 -12 4 -1 -1.08 13.39 12 -4 1 12.15 11.60 -12 -4 -1 -10.16 19.33 -12 -4 -1 10.41 15.51 12 -4 1 -48.15 19.37 12 4 2 13.30 12.56 12 4 2 -0.14 33.38 -12 4 -2 0.99 28.73 -12 4 -2 11.38 28.97 12 -4 2 11.09 15.62 -12 -4 -2 -7.14 23.29 -12 -4 -2 13.56 10.68 12 -4 2 37.60 22.84 12 4 3 10.36 20.08 12 4 3 0.39 16.01 -12 4 -3 -10.93 13.46 -12 -4 -3 16.15 20.31 12 -4 3 -5.66 26.36 13 0 -4 4.38 11.46 13 0 -4 19.08 31.72 -13 0 4 28.22 14.11 -13 0 4 9.81 12.75 13 0 -3 51.89 26.57 13 0 -3 45.28 20.08 -13 0 3 25.39 16.48 -13 0 3 4.69 26.34 13 0 -2 29.11 13.80 13 0 -2 -10.11 17.06 -13 0 2 17.67 15.56 -13 0 2 8.52 13.33 13 0 -1 -0.30 12.92 13 0 -1 5.45 15.43 -13 0 1 -15.51 27.58 -13 0 1 18.89 21.54 13 0 0 -21.78 26.66 13 0 0 27.85 33.58 -13 0 0 20.36 19.26 -13 0 0 26.83 14.25 13 0 1 2.25 14.23 13 0 1 -3.00 17.17 -13 0 -1 24.25 18.13 -13 0 -1 8.06 13.02 13 0 2 1.10 13.79 -13 0 -2 -5.11 17.36 13 1 -3 28.38 14.45 13 1 -3 43.68 16.51 -13 1 3 -7.45 26.96 -13 1 3 37.59 14.74 13 -1 -3 21.94 20.12 -13 -1 3 2.71 24.23 -13 -1 3 16.58 17.15 13 -1 -3 5.96 12.11 13 1 -2 -5.12 21.79 13 1 -2 12.76 13.70 -13 1 2 -0.43 12.23 -13 1 2 -14.82 23.11 13 -1 -2 -2.52 29.35 -13 -1 2 11.69 10.45 -13 -1 2 16.27 14.52 13 -1 -2 -54.35 18.54 13 1 -1 4.35 13.64 13 1 -1 3.14 15.03 -13 1 1 1.57 13.52 -13 1 1 -9.14 26.63 13 -1 -1 6.09 17.48 -13 -1 1 6.31 20.44 -13 -1 1 65.34 30.03 13 -1 -1 7.87 12.34 13 1 0 2.15 14.57 13 1 0 9.91 16.29 -13 1 0 0.56 25.49 -13 1 0 14.11 16.34 13 -1 0 20.31 18.78 -13 -1 0 6.73 12.26 -13 -1 0 18.43 18.02 13 -1 0 9.79 13.62 13 1 1 8.93 15.31 13 1 1 12.87 30.40 -13 1 -1 -2.43 14.29 -13 1 -1 8.00 32.20 13 -1 1 8.27 19.36 -13 -1 -1 14.80 19.67 -13 -1 -1 13.44 12.79 13 -1 1 15.04 13.81 ; _shelx_hkl_checksum 63927 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+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 Br1 Br 0.60807(13) 0.55654(19) 0.32368(8) 0.1035(6) Uani 1 1 d . . Br2 Br 1.62935(14) -0.0439(2) 0.94006(10) 0.1217(7) Uani 1 1 d . . O1 O 0.6210(6) 0.4516(11) 0.7481(5) 0.083(2) Uani 1 1 d . . H1 H 0.634422 0.425010 0.797517 0.099 Uiso 1 1 calc R U O2 O 0.9909(8) 0.1732(10) 0.9765(4) 0.083(2) Uani 1 1 d . . H2A H 0.916090 0.209549 0.971471 0.100 Uiso 1 1 calc R U O33 O 0.8019(8) 0.3090(9) 0.8638(4) 0.080(2) Uani 1 1 d . . C2 C 0.8457(8) 0.3685(9) 0.7215(5) 0.0484(18) Uani 1 1 d . . H2 H 0.895217 0.313369 0.679418 0.058 Uiso 1 1 calc R U C3 C 1.0413(8) 0.5601(10) 0.7403(5) 0.0548(18) Uani 1 1 d . . C4 C 0.6307(9) 0.4934(13) 0.4379(6) 0.070(3) Uani 1 1 d . . C5 C 0.6722(8) 0.4048(10) 0.6068(6) 0.057(2) Uani 1 1 d . . C6 C 0.8930(9) 0.5387(11) 0.7246(6) 0.062(2) Uani 1 1 d . . H6A H 0.865850 0.587959 0.671410 0.074 Uiso 1 1 calc R U H6B H 0.848573 0.591795 0.768909 0.074 Uiso 1 1 calc R U C7 C 1.0050(9) 0.2025(10) 0.8231(5) 0.0535(19) Uani 1 1 d . . H7 H 1.067234 0.236476 0.781674 0.064 Uiso 1 1 calc R U C8 C 0.9206(9) -0.0154(10) 0.7220(6) 0.058(2) Uani 1 1 d . . C9 C 1.2041(10) 0.1658(11) 0.9200(5) 0.059(2) Uani 1 1 d . . C10 C 0.6969(8) 0.3565(10) 0.6952(5) 0.056(2) Uani 1 1 d . . H10 H 0.668719 0.248671 0.700961 0.067 Uiso 1 1 calc R U C11 C 0.7225(10) 0.3190(11) 0.5414(6) 0.061(2) Uani 1 1 d . . H11 H 0.769560 0.228997 0.554711 0.074 Uiso 1 1 calc R U C12 C 1.2351(11) 0.0452(15) 0.9756(6) 0.075(3) Uani 1 1 d . . H12 H 1.170562 0.005540 1.009015 0.090 Uiso 1 1 calc R U C13 C 1.1259(11) 0.5129(13) 0.6829(7) 0.077(3) Uani 1 1 d . . H13 H 1.092875 0.464920 0.633593 0.093 Uiso 1 1 calc R U C14 C 1.0890(11) 0.6328(11) 0.8151(6) 0.066(2) Uani 1 1 d . . H14 H 1.032607 0.664573 0.856162 0.079 Uiso 1 1 calc R U C15 C 0.8774(9) 0.2946(10) 0.8073(5) 0.055(2) Uani 1 1 d . . C16 C 1.0684(10) 0.2324(11) 0.9105(5) 0.061(2) Uani 1 1 d . . H16 H 1.075799 0.344731 0.918052 0.073 Uiso 1 1 calc R U C17 C 1.4588(10) 0.0366(16) 0.9331(6) 0.075(3) Uani 1 1 d . . C18 C 1.3030(11) 0.2252(12) 0.8738(6) 0.067(2) Uani 1 1 d . . H18 H 1.283820 0.308257 0.837840 0.080 Uiso 1 1 calc R U C19 C 0.9774(10) 0.0274(11) 0.8079(6) 0.065(2) Uani 1 1 d . . H19A H 1.059771 -0.028577 0.818216 0.078 Uiso 1 1 calc R U H19B H 0.917101 -0.007644 0.849325 0.078 Uiso 1 1 calc R U C20 C 0.5966(9) 0.5354(13) 0.5845(6) 0.068(2) Uani 1 1 d . . H20 H 0.558376 0.593014 0.626308 0.082 Uiso 1 1 calc R U C21 C 0.7907(11) -0.0528(12) 0.7062(7) 0.074(3) Uani 1 1 d . . H21 H 0.733354 -0.048536 0.750000 0.089 Uiso 1 1 calc R U C22 C 0.7050(10) 0.3627(13) 0.4571(6) 0.071(3) Uani 1 1 d . . H22 H 0.742307 0.305492 0.414843 0.085 Uiso 1 1 calc R U C23 C 0.7423(11) -0.0973(12) 0.6260(7) 0.076(3) Uani 1 1 d . . H23 H 0.654114 -0.126156 0.617459 0.091 Uiso 1 1 calc R U C24 C 0.5781(9) 0.5799(13) 0.5006(7) 0.073(3) Uani 1 1 d . . H24 H 0.529723 0.668719 0.486731 0.088 Uiso 1 1 calc R U C25 C 1.4294(11) 0.1667(13) 0.8788(5) 0.071(3) Uani 1 1 d . . H25 H 1.494809 0.210537 0.847542 0.085 Uiso 1 1 calc R U C26 C 1.0003(10) -0.0177(16) 0.6543(7) 0.085(3) Uani 1 1 d . . H26 H 1.088936 0.009097 0.663154 0.101 Uiso 1 1 calc R U C27 C 0.8208(12) -0.0991(15) 0.5611(7) 0.084(3) Uani 1 1 d . . H27 H 0.787301 -0.127282 0.507442 0.100 Uiso 1 1 calc R U C28 C 1.3602(11) -0.0161(15) 0.9816(7) 0.081(3) Uani 1 1 d . . H28 H 1.378781 -0.096064 1.019711 0.097 Uiso 1 1 calc R U C29 C 0.9535(13) -0.058(2) 0.5745(7) 0.097(4) Uani 1 1 d . . H29 H 1.009498 -0.058540 0.529983 0.116 Uiso 1 1 calc R U C30 C 1.2631(11) 0.5345(15) 0.6959(9) 0.085(3) Uani 1 1 d . . H30 H 1.320378 0.498039 0.656619 0.102 Uiso 1 1 calc R U C31 C 1.3103(12) 0.6081(15) 0.7655(11) 0.099(4) Uani 1 1 d . . H31 H 1.400562 0.627173 0.773260 0.118 Uiso 1 1 calc R U C32 C 1.2274(14) 0.6553(15) 0.8249(9) 0.093(4) Uani 1 1 d . . H32 H 1.262661 0.703861 0.873453 0.111 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 Br1 0.0797(8) 0.1541(13) 0.0756(7) 0.0360(8) -0.0053(5) 0.0161(8) Br2 0.0852(9) 0.1805(17) 0.1001(10) 0.0520(11) 0.0116(7) 0.0322(10) O1 0.056(4) 0.112(6) 0.082(4) 0.016(4) 0.012(3) 0.013(4) O2 0.092(5) 0.105(6) 0.053(4) 0.015(4) 0.012(4) 0.019(4) O33 0.092(5) 0.093(5) 0.055(4) 0.009(4) 0.016(4) 0.023(4) C2 0.044(4) 0.049(4) 0.051(4) 0.005(3) -0.002(3) -0.001(3) C3 0.054(4) 0.051(4) 0.060(4) 0.008(4) -0.001(4) 0.005(4) C4 0.052(5) 0.082(7) 0.074(6) 0.008(5) -0.004(5) 0.001(5) C5 0.048(4) 0.056(5) 0.066(5) 0.008(4) -0.010(4) -0.005(4) C6 0.056(5) 0.055(5) 0.073(5) 0.006(5) -0.003(4) -0.002(4) C7 0.064(5) 0.052(5) 0.045(4) -0.003(4) 0.004(4) 0.006(4) C8 0.059(5) 0.051(4) 0.064(5) -0.004(4) 0.002(4) 0.006(4) C9 0.073(6) 0.065(5) 0.039(4) 0.004(4) -0.009(4) -0.010(5) C10 0.052(5) 0.056(5) 0.059(5) 0.000(4) 0.002(4) -0.005(4) C11 0.068(6) 0.056(5) 0.060(5) 0.007(4) 0.002(4) 0.000(4) C12 0.085(7) 0.085(6) 0.054(5) 0.032(5) -0.003(4) 0.000(6) C13 0.082(7) 0.088(8) 0.062(5) 0.009(5) 0.010(5) -0.003(5) C14 0.075(6) 0.052(5) 0.070(6) -0.003(4) -0.002(5) 0.001(4) C15 0.064(5) 0.048(4) 0.052(5) -0.002(4) 0.008(4) 0.005(4) C16 0.075(6) 0.068(5) 0.040(4) 0.004(4) -0.007(4) 0.005(5) C17 0.067(5) 0.108(8) 0.049(4) 0.009(5) 0.002(4) 0.001(6) C18 0.080(7) 0.072(6) 0.048(5) 0.010(4) -0.007(4) -0.010(5) C19 0.074(6) 0.058(5) 0.062(5) 0.001(4) -0.014(4) -0.002(5) C20 0.058(5) 0.078(6) 0.069(5) 0.005(5) 0.003(4) 0.011(5) C21 0.078(6) 0.060(6) 0.082(7) -0.003(5) -0.005(5) -0.010(5) C22 0.064(6) 0.079(7) 0.069(6) -0.006(5) -0.001(5) 0.007(5) C23 0.063(6) 0.070(6) 0.092(7) -0.011(5) -0.007(6) 0.001(5) C24 0.060(5) 0.073(6) 0.084(7) 0.022(5) -0.009(5) 0.016(5) C25 0.082(7) 0.090(7) 0.041(4) 0.010(5) -0.003(4) -0.019(6) C26 0.058(5) 0.117(9) 0.080(7) -0.031(7) 0.012(5) 0.001(6) C27 0.088(8) 0.095(8) 0.065(6) -0.018(6) -0.013(6) 0.006(6) C28 0.074(6) 0.099(8) 0.068(6) 0.030(6) -0.008(5) 0.002(6) C29 0.087(8) 0.142(11) 0.061(6) -0.027(7) 0.004(6) 0.002(8) C30 0.062(6) 0.084(8) 0.112(9) 0.016(7) 0.025(6) -0.007(6) C31 0.063(7) 0.084(8) 0.147(13) 0.038(9) -0.005(8) -0.016(6) C32 0.088(9) 0.080(7) 0.106(9) 0.000(7) -0.030(8) -0.010(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Br Br -0.2901 2.4595 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 C10 O1 H1 109.5 C16 O2 H2A 109.5 C15 C2 C10 111.5(7) C15 C2 C6 108.7(7) C10 C2 C6 111.6(7) C15 C2 H2 108.3 C10 C2 H2 108.3 C6 C2 H2 108.3 C13 C3 C14 120.3(9) C13 C3 C6 120.8(9) C14 C3 C6 118.9(8) C24 C4 C22 120.8(9) C24 C4 Br1 120.3(7) C22 C4 Br1 118.9(8) C11 C5 C20 117.3(8) C11 C5 C10 120.6(8) C20 C5 C10 122.1(9) C3 C6 C2 115.0(7) C3 C6 H6A 108.5 C2 C6 H6A 108.5 C3 C6 H6B 108.5 C2 C6 H6B 108.5 H6A C6 H6B 107.5 C16 C7 C15 111.8(7) C16 C7 C19 111.7(7) C15 C7 C19 109.8(8) C16 C7 H7 107.8 C15 C7 H7 107.8 C19 C7 H7 107.8 C21 C8 C26 117.1(10) C21 C8 C19 122.9(9) C26 C8 C19 119.9(9) C18 C9 C12 118.1(10) C18 C9 C16 119.9(8) C12 C9 C16 121.9(9) O1 C10 C5 109.1(7) O1 C10 C2 110.7(7) C5 C10 C2 110.4(7) O1 C10 H10 108.9 C5 C10 H10 108.9 C2 C10 H10 108.9 C22 C11 C5 122.6(9) C22 C11 H11 118.7 C5 C11 H11 118.7 C28 C12 C9 120.6(9) C28 C12 H12 119.7 C9 C12 H12 119.7 C3 C13 C30 121.4(11) C3 C13 H13 119.3 C30 C13 H13 119.3 C3 C14 C32 116.4(10) C3 C14 H14 121.8 C32 C14 H14 121.8 O33 C15 C2 120.3(8) O33 C15 C7 119.7(8) C2 C15 C7 120.0(7) O2 C16 C9 109.2(7) O2 C16 C7 112.6(8) C9 C16 C7 111.5(7) O2 C16 H16 107.8 C9 C16 H16 107.8 C7 C16 H16 107.8 C28 C17 C25 117.6(10) C28 C17 Br2 123.1(9) C25 C17 Br2 119.2(8) C9 C18 C25 122.5(9) C9 C18 H18 118.7 C25 C18 H18 118.7 C8 C19 C7 116.0(7) C8 C19 H19A 108.3 C7 C19 H19A 108.3 C8 C19 H19B 108.3 C7 C19 H19B 108.3 H19A C19 H19B 107.4 C24 C20 C5 120.6(9) C24 C20 H20 119.7 C5 C20 H20 119.7 C8 C21 C23 121.3(11) C8 C21 H21 119.4 C23 C21 H21 119.4 C4 C22 C11 118.2(10) C4 C22 H22 120.9 C11 C22 H22 120.9 C27 C23 C21 120.9(11) C27 C23 H23 119.6 C21 C23 H23 119.6 C4 C24 C20 120.4(9) C4 C24 H24 119.8 C20 C24 H24 119.8 C18 C25 C17 118.9(9) C18 C25 H25 120.6 C17 C25 H25 120.6 C29 C26 C8 122.3(11) C29 C26 H26 118.9 C8 C26 H26 118.9 C23 C27 C29 119.4(10) C23 C27 H27 120.3 C29 C27 H27 120.3 C17 C28 C12 122.1(10) C17 C28 H28 118.9 C12 C28 H28 118.9 C26 C29 C27 119.1(10) C26 C29 H29 120.5 C27 C29 H29 120.5 C31 C30 C13 119.3(11) C31 C30 H30 120.4 C13 C30 H30 120.4 C30 C31 C32 120.4(11) C30 C31 H31 119.8 C32 C31 H31 119.8 C31 C32 C14 122.1(12) C31 C32 H32 119.0 C14 C32 H32 119.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C4 1.891(10) Br2 C17 1.861(11) O1 C10 1.428(12) O1 H1 0.8200 O2 C16 1.436(12) O2 H2A 0.8200 O33 C15 1.215(10) C2 C15 1.520(12) C2 C10 1.544(12) C2 C6 1.546(12) C2 H2 0.9800 C3 C13 1.348(13) C3 C14 1.403(13) C3 C6 1.520(12) C4 C24 1.376(15) C4 C22 1.381(15) C5 C11 1.394(13) C5 C20 1.398(14) C5 C10 1.469(12) C6 H6A 0.9700 C6 H6B 0.9700 C7 C16 1.516(12) C7 C15 1.526(12) C7 C19 1.554(13) C7 H7 0.9800 C8 C21 1.364(14) C8 C26 1.378(14) C8 C19 1.495(13) C9 C18 1.373(14) C9 C12 1.389(13) C9 C16 1.490(14) C10 H10 0.9800 C11 C22 1.389(13) C11 H11 0.9300 C12 C28 1.371(15) C12 H12 0.9300 C13 C30 1.406(16) C13 H13 0.9300 C14 C32 1.415(17) C14 H14 0.9300 C16 H16 0.9800 C17 C28 1.371(14) C17 C25 1.436(16) C18 C25 1.375(16) C18 H18 0.9300 C19 H19A 0.9700 C19 H19B 0.9700 C20 C24 1.385(14) C20 H20 0.9300 C21 C23 1.390(15) C21 H21 0.9300 C22 H22 0.9300 C23 C27 1.335(16) C23 H23 0.9300 C24 H24 0.9300 C25 H25 0.9300 C26 C29 1.370(15) C26 H26 0.9300 C27 C29 1.395(17) C27 H27 0.9300 C28 H28 0.9300 C29 H29 0.9300 C30 C31 1.337(19) C30 H30 0.9300 C31 C32 1.359(19) C31 H31 0.9300 C32 H32 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1 O33 2.803(10) 0.820 2.187 132.0 no O2 H2A O33 2.801(11) 0.820 2.183 132.2 no 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 C13 C3 C6 C2 65.8(12) C14 C3 C6 C2 -115.3(9) C15 C2 C6 C3 63.1(10) C10 C2 C6 C3 -173.5(7) C11 C5 C10 O1 -172.5(8) C20 C5 C10 O1 6.4(11) C11 C5 C10 C2 65.6(10) C20 C5 C10 C2 -115.5(9) C15 C2 C10 O1 68.5(9) C6 C2 C10 O1 -53.3(10) C15 C2 C10 C5 -170.6(7) C6 C2 C10 C5 67.6(10) C20 C5 C11 C22 3.0(14) C10 C5 C11 C22 -178.1(9) C18 C9 C12 C28 -2.3(16) C16 C9 C12 C28 178.5(11) C14 C3 C13 C30 0.0(15) C6 C3 C13 C30 178.8(9) C13 C3 C14 C32 1.3(14) C6 C3 C14 C32 -177.5(9) C10 C2 C15 O33 -38.8(12) C6 C2 C15 O33 84.7(10) C10 C2 C15 C7 141.5(8) C6 C2 C15 C7 -95.0(9) C16 C7 C15 O33 -39.5(12) C19 C7 C15 O33 85.1(10) C16 C7 C15 C2 140.2(8) C19 C7 C15 C2 -95.2(9) C18 C9 C16 O2 -168.5(8) C12 C9 C16 O2 10.6(13) C18 C9 C16 C7 66.4(12) C12 C9 C16 C7 -114.4(10) C15 C7 C16 O2 67.3(10) C19 C7 C16 O2 -56.2(10) C15 C7 C16 C9 -169.6(8) C19 C7 C16 C9 66.9(10) C12 C9 C18 C25 2.0(15) C16 C9 C18 C25 -178.8(9) C21 C8 C19 C7 -104.1(11) C26 C8 C19 C7 75.7(13) C16 C7 C19 C8 -177.3(8) C15 C7 C19 C8 58.0(11) C11 C5 C20 C24 -2.7(14) C10 C5 C20 C24 178.4(9) C26 C8 C21 C23 2.5(16) C19 C8 C21 C23 -177.7(9) C24 C4 C22 C11 1.5(15) Br1 C4 C22 C11 179.0(8) C5 C11 C22 C4 -2.4(15) C8 C21 C23 C27 -2.5(17) C22 C4 C24 C20 -1.3(16) Br1 C4 C24 C20 -178.8(8) C5 C20 C24 C4 1.9(16) C9 C18 C25 C17 1.2(16) C28 C17 C25 C18 -4.1(16) Br2 C17 C25 C18 179.8(8) C21 C8 C26 C29 -1.1(19) C19 C8 C26 C29 179.1(12) C21 C23 C27 C29 1.1(19) C25 C17 C28 C12 3.9(18) Br2 C17 C28 C12 179.9(10) C9 C12 C28 C17 -0.7(19) C8 C26 C29 C27 0(2) C23 C27 C29 C26 0(2) C3 C13 C30 C31 -2.2(17) C13 C30 C31 C32 3.0(18) C30 C31 C32 C14 -2(2) C3 C14 C32 C31 -0.5(17)