#------------------------------------------------------------------------------ #$Date: 2021-07-07 06:41:49 +0300 (Wed, 07 Jul 2021) $ #$Revision: 267319 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158165.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_7158165 loop_ _publ_author_name 'Zhao, Gang' 'Fang, Guo-Sheng' 'Wang, Hongyu' 'Zheng, Changwu' 'Pan, Lu' _publ_section_title ; Enantioselective Switch in Asymmetric Michael Addition Reactions using Phosphonium Salts ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01027A _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_sum 'C39 H32 Br F12 N2 O2 P' _chemical_formula_weight 899.54 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2013 _audit_update_record ; 2019-02-14 deposited with the CCDC. 2021-06-28 downloaded from the CCDC. ; _cell_angle_alpha 72.036(2) _cell_angle_beta 88.944(2) _cell_angle_gamma 84.345(2) _cell_formula_units_Z 2 _cell_length_a 8.7747(4) _cell_length_b 15.1721(9) _cell_length_c 16.4580(9) _cell_measurement_reflns_used 6842 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 51.366 _cell_measurement_theta_min 4.400 _cell_volume 2073.94(19) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_unetI/netI 0.1686 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 31904 _diffrn_reflns_point_group_measured_fraction_full 0.943 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 24.998 _diffrn_reflns_theta_min 2.333 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_T_max 0.7153 _exptl_absorpt_correction_T_min 0.5531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.440 _exptl_crystal_description prismatic _exptl_crystal_F_000 908 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.702 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.101 _refine_ls_abs_structure_details ; Flack x determined using 2872 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.187(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1079 _refine_ls_number_reflns 14162 _refine_ls_number_restraints 186 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.1053 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1897P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2673 _refine_ls_wR_factor_ref 0.3269 _reflns_Friedel_coverage 0.943 _reflns_Friedel_fraction_full 0.915 _reflns_Friedel_fraction_max 0.940 _reflns_number_gt 8305 _reflns_number_total 14162 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01027a2.cif _cod_data_source_block mo_d8v18672_0m _cod_database_code 7158165 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.816 _shelx_estimated_absorpt_t_max 0.916 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_d8v18672_0m_a.res in P1 CELL 0.71073 8.7747 15.1721 16.458 72.036 88.944 84.345 ZERR 2 0.0004 0.0009 0.0009 0.002 0.002 0.002 LATT -1 SFAC C H N O F P Br UNIT 78 64 4 4 24 2 2 OMIT 0 1 0 OMIT 0 -1 -1 OMIT 0 1 1 OMIT -3.00 50.00 L.S. 7 ACTA BOND $H FMAP 2 PLAN 20 LIST 4 htab conf mpla wpdb -1 size 0.19 0.13 0.08 DFIX 1.45 C13 C17 C15 C18 C34 C39 C36 C38 DFIX 1.45 C73 C77 C75 C78 C15 C18' dfix 1.33 0.02 c18' f4' c18' f5' c18' f6' c18 f4 c18 f5 c18 f6 DFIX 1.33 C77 F19 C77 F20 C77 F21 C78 F22 C78 F23 C78 F24 DFIX 1.33 C38 F7 C38 F8 C38 F9 C39 F10 C39 F11 C39 F12 SIMU 0.004 0.008 2 C17 C18 C38 C39 C77 C78 C46 C18 C28 SIMU 0.004 0.008 2 F16 F17 F18 F19 F20 F21 F22 F23 F24 SIMU 0.003 0.006 2 F1 F2 F3 F4 F5 F6 F7 F8 F9 F10 F11 F12 F13 F14 F15 SIMU 0.004 0.008 2 F4' F5' F6' C18' F10' F11' F12' dfix 2.35 0.02 c14 c18' ISOR 0.01 0.02 C78 C46 C47 c18 c18' c4 c5 c6 c7 c45 c39 f11' delu 0.003 c15 c18' TEMP 23 WGHT 0.189700 EXTI 0.016213 FVAR 0.73723 BR1 7 0.698292 0.880680 0.049673 11.00000 0.11171 0.23107 = 0.08186 -0.08708 -0.00201 -0.00465 BR2 7 0.175246 0.114465 0.922812 11.00000 0.14641 0.22433 = 0.08623 -0.08853 0.03546 -0.05475 P1 6 0.506334 0.976535 0.255635 11.00000 0.06210 0.06220 = 0.05237 -0.02273 0.00015 -0.00971 P2 6 0.979650 0.025998 0.718183 11.00000 0.05543 0.05676 = 0.04793 -0.01849 0.00006 -0.00241 N1 3 0.166683 0.993098 0.157959 11.00000 0.06239 0.08156 = 0.04573 -0.02025 -0.00218 0.00181 AFIX 43 H1 2 0.194938 1.001302 0.106047 11.00000 -1.20000 AFIX 0 N2 3 0.027508 1.132052 0.105856 11.00000 0.09235 0.08449 = 0.04589 -0.02171 -0.00059 0.02143 AFIX 43 H2 2 0.060742 1.127510 0.057682 11.00000 -1.20000 AFIX 0 N3 3 0.649515 -0.002884 0.819868 11.00000 0.07715 0.06736 = 0.04498 -0.02212 -0.00063 -0.01198 AFIX 43 H3 2 0.689740 -0.016586 0.870023 11.00000 -1.20000 AFIX 0 N4 3 0.546053 -0.139208 0.870957 11.00000 0.10473 0.07764 = 0.04309 -0.02057 0.00327 -0.02969 AFIX 43 H4 2 0.582882 -0.138193 0.918690 11.00000 -1.20000 AFIX 0 O1 4 0.022430 1.049981 0.248371 11.00000 0.08225 0.07978 = 0.04140 -0.02241 0.01147 -0.00045 O2 4 0.512373 -0.053001 0.730599 11.00000 0.07891 0.07289 = 0.05043 -0.01555 -0.00478 -0.01697 AFIX 6 O3 4 0.330283 0.920199 0.017795 11.00000 0.20866 0.24379 = 0.14267 -0.04985 0.02143 0.00162 H3C 2 0.339874 0.862420 0.045262 11.00000 -1.50000 H3D 2 0.313933 0.922460 -0.033588 11.00000 -1.50000 O4 4 0.821887 0.074352 0.956613 11.00000 0.24540 0.33487 = 0.09796 -0.05855 0.00243 -0.05447 H4A 2 0.833151 0.033691 1.005500 11.00000 -1.50000 H4B 2 0.741087 0.108426 0.960774 11.00000 -1.50000 AFIX 0 C1 1 0.403661 0.896881 0.221585 11.00000 0.04862 0.06054 = 0.05733 -0.02464 -0.00035 0.00151 AFIX 23 H1A 2 0.432465 0.901929 0.163254 11.00000 -1.20000 H1B 2 0.438195 0.834170 0.256633 11.00000 -1.20000 AFIX 0 C2 1 0.229361 0.908892 0.224838 11.00000 0.05790 0.06429 = 0.05482 -0.02244 0.00269 -0.00846 AFIX 13 H2A 2 0.200595 0.916213 0.280385 11.00000 -1.20000 AFIX 0 C3 1 0.162609 0.822768 0.217723 11.00000 0.05798 0.08698 = 0.08888 -0.03394 0.00696 -0.02242 AFIX 23 H3A 2 0.051720 0.832232 0.218657 11.00000 -1.20000 H3B 2 0.191815 0.813400 0.163630 11.00000 -1.20000 AFIX 0 C4 1 0.217776 0.737460 0.289545 11.00000 0.06818 0.07537 = 0.12647 -0.02969 0.00435 -0.01912 C5 1 0.315771 0.665151 0.283993 11.00000 0.11369 0.09829 = 0.14620 -0.01965 0.02714 -0.00449 AFIX 43 H5 2 0.357270 0.669030 0.230738 11.00000 -1.20000 AFIX 0 C6 1 0.360140 0.584940 0.351523 11.00000 0.14682 0.12867 = 0.17515 -0.04123 -0.00187 0.00435 AFIX 43 H6 2 0.408987 0.531761 0.342134 11.00000 -1.20000 AFIX 0 C7 1 0.330725 0.588410 0.425239 11.00000 0.12000 0.11265 = 0.15300 -0.00774 -0.00915 -0.00625 AFIX 43 H7 2 0.379437 0.542141 0.470753 11.00000 -1.20000 AFIX 0 C8 1 0.227454 0.658395 0.444988 11.00000 0.10194 0.11981 = 0.17163 0.03757 -0.00354 -0.02975 AFIX 43 H8 2 0.199539 0.656134 0.500329 11.00000 -1.20000 AFIX 0 C9 1 0.173074 0.730499 0.372153 11.00000 0.08559 0.08561 = 0.10224 -0.00115 0.01408 -0.02615 AFIX 43 H9 2 0.102068 0.776798 0.379984 11.00000 -1.20000 AFIX 0 C10 1 0.067321 1.057207 0.175270 11.00000 0.06600 0.06084 = 0.05572 -0.02198 -0.00287 0.00521 C11 1 -0.060064 1.215268 0.102292 11.00000 0.08361 0.07204 = 0.04522 -0.02082 -0.00653 0.00024 C12 1 -0.130016 1.230161 0.175137 11.00000 0.09844 0.05878 = 0.07046 -0.00859 -0.00424 0.01454 AFIX 43 H12 2 -0.121361 1.184052 0.227826 11.00000 -1.20000 AFIX 0 C13 1 -0.213655 1.317001 0.166012 11.00000 0.09256 0.08084 = 0.09130 -0.04142 -0.00562 0.00074 C14 1 -0.225160 1.385825 0.089432 11.00000 0.14823 0.06062 = 0.07590 -0.00613 -0.00838 0.01533 PART 1 AFIX 43 H14 2 -0.283218 1.441957 0.084518 11.00000 -1.20000 PART 0 AFIX 0 C15 1 -0.149768 1.371746 0.018749 11.00000 0.16489 0.08153 = 0.08789 -0.02175 0.03717 -0.03891 C16 1 -0.068468 1.285249 0.025726 11.00000 0.12192 0.07389 = 0.05952 -0.00669 0.01251 0.01126 AFIX 43 H16 2 -0.019975 1.275294 -0.021847 11.00000 -1.20000 AFIX 0 C17 1 -0.296561 1.328729 0.242232 11.00000 0.14654 0.09103 = 0.07680 -0.03542 -0.00842 0.03979 C19 1 0.462542 0.969493 0.363747 11.00000 0.07253 0.08027 = 0.05498 -0.02645 0.00064 -0.00023 C20 1 0.406117 0.890835 0.417318 11.00000 0.08553 0.09300 = 0.05177 -0.02638 0.00134 -0.00759 AFIX 43 H20 2 0.374406 0.847348 0.393563 11.00000 -1.20000 AFIX 0 C21 1 0.394569 0.873743 0.502676 11.00000 0.09467 0.14449 = 0.05173 0.00172 -0.00316 0.00687 AFIX 43 H21 2 0.358209 0.819187 0.537188 11.00000 -1.20000 AFIX 0 C22 1 0.438313 0.939618 0.536962 11.00000 0.11610 0.16238 = 0.04857 -0.03525 0.01258 0.01228 AFIX 43 H22 2 0.428918 0.930298 0.595321 11.00000 -1.20000 AFIX 0 C23 1 0.494340 1.017104 0.487140 11.00000 0.08793 0.22307 = 0.08692 -0.09445 -0.02133 0.01234 AFIX 43 H23 2 0.523361 1.060345 0.511995 11.00000 -1.20000 AFIX 0 C24 1 0.510391 1.034793 0.399312 11.00000 0.08495 0.11283 = 0.07965 -0.05766 -0.00266 -0.02204 AFIX 43 H24 2 0.551450 1.088113 0.365641 11.00000 -1.20000 AFIX 0 C25 1 0.470742 1.091386 0.186570 11.00000 0.07902 0.06200 = 0.06693 -0.01972 -0.01723 -0.01483 C26 1 0.366673 1.156754 0.205628 11.00000 0.10079 0.07914 = 0.11865 -0.03375 -0.02737 -0.00585 AFIX 43 H26 2 0.314734 1.141649 0.257117 11.00000 -1.20000 AFIX 0 C27 1 0.340210 1.246802 0.145894 11.00000 0.13095 0.06447 = 0.17419 -0.01606 -0.05514 0.00380 AFIX 43 H27 2 0.276203 1.292852 0.159259 11.00000 -1.20000 AFIX 0 C28 1 0.409868 1.265112 0.068462 11.00000 0.19924 0.04790 = 0.19458 0.00777 -0.06273 -0.01576 AFIX 43 H28 2 0.385074 1.322693 0.027859 11.00000 -1.20000 AFIX 0 C29 1 0.511921 1.204242 0.048282 11.00000 0.29509 0.07371 = 0.07522 0.01454 -0.05206 -0.03846 AFIX 43 H29 2 0.559973 1.220278 -0.004382 11.00000 -1.20000 AFIX 0 C30 1 0.545373 1.116701 0.106934 11.00000 0.13683 0.09817 = 0.07107 -0.02226 0.00245 -0.00953 AFIX 43 H30 2 0.617613 1.074215 0.093764 11.00000 -1.20000 AFIX 0 C31 1 0.706841 0.937733 0.256202 11.00000 0.06006 0.08429 = 0.05696 -0.02548 -0.00161 -0.01422 AFIX 23 H31A 2 0.736458 0.938608 0.198904 11.00000 -1.20000 H31B 2 0.765467 0.980808 0.272355 11.00000 -1.20000 AFIX 0 C32 1 0.746450 0.840388 0.317141 11.00000 0.05393 0.08086 = 0.07278 -0.03570 0.00351 -0.01768 C33 1 0.761405 0.764422 0.286688 11.00000 0.06122 0.07521 = 0.09272 -0.04383 -0.00328 -0.00443 AFIX 43 H33 2 0.746324 0.771804 0.229089 11.00000 -1.20000 AFIX 0 C37 1 0.768960 0.827802 0.402845 11.00000 0.07355 0.06798 = 0.07970 -0.02273 -0.01221 -0.00424 AFIX 43 H37 2 0.762599 0.879112 0.422769 11.00000 -1.20000 AFIX 0 C36 1 0.800712 0.739902 0.458894 11.00000 0.06003 0.09337 = 0.08723 -0.03200 -0.01247 -0.00565 C40 1 0.847334 0.102836 0.754760 11.00000 0.04993 0.06859 = 0.05588 -0.02708 0.00535 -0.00589 AFIX 23 H40A 2 0.877608 0.098757 0.812295 11.00000 -1.20000 H40B 2 0.857545 0.166016 0.718933 11.00000 -1.20000 AFIX 0 C41 1 0.676485 0.086093 0.755811 11.00000 0.04908 0.07035 = 0.04578 -0.01324 0.00242 -0.01143 AFIX 13 H41 2 0.649205 0.082527 0.699512 11.00000 -1.20000 AFIX 0 C42 1 0.577486 0.168000 0.771158 11.00000 0.04495 0.07621 = 0.11523 -0.02011 0.01022 -0.00307 AFIX 23 H42A 2 0.471232 0.154830 0.773846 11.00000 -1.20000 H42B 2 0.605276 0.172825 0.826294 11.00000 -1.20000 AFIX 66 C43 1 0.590527 0.257290 0.706764 11.00000 0.04869 0.07599 = 0.14511 -0.00999 -0.00238 0.00902 C44 1 0.563349 0.269261 0.620907 11.00000 0.06210 0.08533 = 0.14661 -0.00328 0.00214 0.00702 AFIX 43 H44 2 0.529956 0.220978 0.604363 11.00000 -1.20000 AFIX 65 C45 1 0.586082 0.353397 0.559776 11.00000 0.11100 0.12905 = 0.14430 -0.00372 0.00199 -0.00392 AFIX 43 H45 2 0.567898 0.361407 0.502333 11.00000 -1.20000 AFIX 65 C46 1 0.635992 0.425562 0.584502 11.00000 0.13636 0.13014 = 0.15580 -0.01446 -0.00381 -0.02435 AFIX 43 H46 2 0.651202 0.481855 0.543601 11.00000 -1.20000 AFIX 65 C47 1 0.663170 0.413592 0.670358 11.00000 0.17407 0.17164 = 0.20444 -0.05666 -0.00864 -0.03392 AFIX 43 H47 2 0.696563 0.461875 0.686901 11.00000 -1.20000 AFIX 65 C48 1 0.640438 0.329456 0.731490 11.00000 0.13922 0.05697 = 0.22876 -0.03270 -0.04189 -0.00585 AFIX 43 H48 2 0.658622 0.321447 0.788934 11.00000 -1.20000 AFIX 0 C49 1 0.564198 -0.062817 0.802051 11.00000 0.06099 0.06974 = 0.04812 -0.02102 0.00963 -0.00068 C50 1 0.475868 -0.218023 0.873621 11.00000 0.07195 0.07203 = 0.06091 -0.02354 -0.00076 -0.01218 C51 1 0.453111 -0.281419 0.954855 11.00000 0.09735 0.06155 = 0.06628 -0.01068 -0.00038 -0.00735 AFIX 43 H51 2 0.484870 -0.269119 1.003529 11.00000 -1.20000 AFIX 0 C52 1 0.386469 -0.358885 0.962602 11.00000 0.10984 0.05235 = 0.09041 -0.00919 0.00698 -0.00315 C53 1 0.338016 -0.381818 0.892494 11.00000 0.13067 0.04962 = 0.11063 -0.01823 0.02193 -0.02176 AFIX 43 H53 2 0.296386 -0.437631 0.899126 11.00000 -1.20000 AFIX 0 C54 1 0.353999 -0.318161 0.811749 11.00000 0.11122 0.09719 = 0.06894 -0.03763 0.00344 -0.01808 C55 1 0.423714 -0.238080 0.802882 11.00000 0.09893 0.07014 = 0.06510 -0.03121 0.00870 -0.02883 AFIX 43 H55 2 0.435899 -0.196924 0.748604 11.00000 -1.20000 AFIX 0 C56 1 0.354983 -0.425070 1.045273 11.00000 0.16129 0.08242 = 0.08270 0.00591 0.00233 -0.00641 C57 1 0.297763 -0.333948 0.734504 11.00000 0.16604 0.10018 = 0.11347 -0.06302 0.04448 -0.05429 C58 1 0.981718 -0.089968 0.786345 11.00000 0.07428 0.05672 = 0.06095 -0.01904 0.00535 -0.00643 C59 1 1.051231 -0.111779 0.866693 11.00000 0.13073 0.06633 = 0.07226 -0.00807 -0.01701 0.01195 AFIX 43 H59 2 1.101781 -0.068251 0.882264 11.00000 -1.20000 AFIX 0 C60 1 1.042260 -0.199492 0.921654 11.00000 0.14325 0.05587 = 0.10972 0.00038 -0.00248 -0.00318 AFIX 43 H60 2 1.095491 -0.214601 0.973237 11.00000 -1.20000 AFIX 0 C61 1 0.971910 -0.259652 0.909993 11.00000 0.15425 0.06097 = 0.11542 0.03081 0.04291 0.01845 AFIX 43 H61 2 0.965223 -0.315422 0.953384 11.00000 -1.20000 AFIX 0 C62 1 0.900228 -0.244203 0.829873 11.00000 0.13330 0.06755 = 0.15788 -0.02646 0.04742 -0.01257 AFIX 43 H62 2 0.852118 -0.291038 0.818308 11.00000 -1.20000 AFIX 0 C63 1 0.903375 -0.153822 0.766204 11.00000 0.08948 0.06448 = 0.10677 -0.03705 -0.00079 0.00091 AFIX 43 H63 2 0.853872 -0.139905 0.713634 11.00000 -1.20000 AFIX 0 C64 1 0.937412 0.034083 0.608888 11.00000 0.05932 0.08454 = 0.05558 -0.02952 0.00742 -0.02105 C65 1 1.012408 -0.025948 0.572042 11.00000 0.08697 0.10740 = 0.07103 -0.04590 0.01843 -0.02369 AFIX 43 H65 2 1.074565 -0.077287 0.604992 11.00000 -1.20000 AFIX 0 C66 1 0.995550 -0.010022 0.482962 11.00000 0.10451 0.15558 = 0.11196 -0.09661 0.03233 -0.03492 AFIX 43 H66 2 1.034037 -0.055379 0.458745 11.00000 -1.20000 AFIX 0 C67 1 0.927448 0.066686 0.435964 11.00000 0.08382 0.19071 = 0.07513 -0.05534 0.00570 -0.01596 AFIX 43 H67 2 0.930857 0.080640 0.376866 11.00000 -1.20000 AFIX 0 C68 1 0.851680 0.127048 0.469944 11.00000 0.09577 0.23193 = 0.05083 -0.03929 -0.00121 -0.02644 AFIX 43 H68 2 0.793604 0.178863 0.434693 11.00000 -1.20000 AFIX 0 C69 1 0.858290 0.113438 0.559167 11.00000 0.07497 0.08584 = 0.05360 -0.01616 -0.01126 0.00283 AFIX 43 H69 2 0.810314 0.157148 0.582724 11.00000 -1.20000 AFIX 0 C70 1 1.165481 0.066785 0.718879 11.00000 0.05355 0.07339 = 0.05146 -0.02578 0.00555 -0.00422 AFIX 23 H70A 2 1.189645 0.066195 0.776331 11.00000 -1.20000 H70B 2 1.241891 0.024499 0.703049 11.00000 -1.20000 AFIX 0 C71 1 1.173712 0.164568 0.657959 11.00000 0.05195 0.06348 = 0.06439 -0.01713 0.00604 -0.00903 C72 1 1.200973 0.179210 0.571349 11.00000 0.08129 0.06896 = 0.06801 -0.02493 0.01001 -0.00836 AFIX 43 H72 2 1.220092 0.128324 0.551180 11.00000 -1.20000 AFIX 0 C73 1 1.200041 0.267397 0.515472 11.00000 0.09196 0.06677 = 0.07219 -0.01095 0.01672 -0.02314 C74 1 1.176076 0.345933 0.542779 11.00000 0.07152 0.08823 = 0.12335 -0.03658 0.01510 -0.00555 AFIX 43 H74 2 1.178591 0.405773 0.505150 11.00000 -1.20000 AFIX 0 C75 1 1.148653 0.330194 0.627953 11.00000 0.06306 0.08094 = 0.10810 -0.04463 0.01281 -0.01261 C76 1 1.146337 0.239735 0.687109 11.00000 0.06482 0.07616 = 0.07683 -0.02425 0.01673 -0.00687 AFIX 43 H76 2 1.126606 0.231751 0.744519 11.00000 -1.20000 AFIX 0 C77 1 1.232358 0.281381 0.429337 11.00000 0.11635 0.14936 = 0.10346 -0.02790 0.04544 -0.05510 C78 1 1.128703 0.408627 0.660959 11.00000 0.09717 0.08116 = 0.14579 -0.03644 0.01905 -0.01643 F1 5 -0.354655 1.256950 0.291736 11.00000 0.13820 0.12910 = 0.10470 -0.04301 0.02805 0.00564 F2 5 -0.190610 1.342375 0.299064 11.00000 0.22042 0.22321 = 0.11605 -0.09519 0.02335 -0.06893 F3 5 -0.389674 1.403881 0.226945 11.00000 0.35555 0.16657 = 0.08214 -0.00922 0.01890 0.15751 PART 1 C18 1 -0.148950 1.445456 -0.063904 10.60000 0.12773 0.09978 = 0.10563 -0.03268 0.02883 0.00235 F4 5 -0.253230 1.518131 -0.075477 10.50000 0.32828 0.09598 = 0.07518 0.01490 -0.05204 0.08904 F5 5 -0.179189 1.417668 -0.131136 10.50000 0.23689 0.12807 = 0.07580 -0.01234 -0.02411 -0.01417 F6 5 -0.017968 1.482844 -0.079569 10.50000 0.28619 0.18603 = 0.16290 0.05638 -0.00355 -0.14650 PART 2 C18' 1 -0.203857 1.442262 -0.060649 10.40000 0.18440 0.14271 = 0.14325 -0.00285 -0.00722 -0.00626 F4' 5 -0.339436 1.438665 -0.094200 10.50000 0.20075 0.15077 = 0.15229 0.00525 -0.01519 -0.00371 F5' 5 -0.090371 1.440709 -0.115161 10.50000 0.18389 0.14495 = 0.13938 0.00326 0.01087 -0.00318 F6' 5 -0.195444 1.523591 -0.045537 10.50000 0.19312 0.13706 = 0.14932 -0.00361 -0.01079 -0.01411 PART 0 F7 5 0.822339 0.649051 0.600166 11.00000 0.42032 0.16606 = 0.09375 -0.01704 -0.03725 -0.02505 F9 5 0.761514 0.792079 0.578241 11.00000 0.40675 0.17172 = 0.08798 -0.04276 -0.05634 0.00561 F13 5 0.459071 -0.424700 1.106504 11.00000 0.31390 0.12647 = 0.11232 0.02727 -0.02026 -0.03023 F14 5 0.238755 -0.395149 1.084636 11.00000 0.30829 0.14807 = 0.11566 0.04213 -0.00040 -0.02150 F15 5 0.373780 -0.508376 1.055657 11.00000 0.32454 0.10775 = 0.12929 0.01865 -0.01905 -0.04397 F16 5 0.191560 -0.393360 0.748667 11.00000 0.23034 0.17305 = 0.15583 -0.06976 -0.01394 -0.09558 F17 5 0.410113 -0.351262 0.684884 11.00000 0.23259 0.20719 = 0.15209 -0.10116 -0.00248 -0.03158 F18 5 0.230749 -0.264697 0.679217 11.00000 0.22505 0.18278 = 0.13723 -0.07752 -0.02124 -0.06317 F19 5 1.194849 0.221271 0.393392 11.00000 0.32503 0.21662 = 0.10294 -0.06926 0.07337 -0.07113 F20 5 1.380957 0.267761 0.411811 11.00000 0.33155 0.23544 = 0.12544 -0.04494 0.08637 -0.04430 F21 5 1.218670 0.360740 0.377584 11.00000 0.35215 0.20824 = 0.12408 -0.02242 0.08101 -0.02895 F22 5 1.255834 0.450380 0.660262 11.00000 0.25892 0.16380 = 0.34181 -0.16672 0.05528 -0.02413 F23 5 1.047290 0.482850 0.607070 11.00000 0.26861 0.15077 = 0.34267 -0.14138 0.05587 0.01403 F24 5 1.057198 0.402494 0.728595 11.00000 0.40484 0.10813 = 0.20727 -0.09330 0.16006 -0.06878 C34 1 0.800594 0.674637 0.346294 11.00000 0.05292 0.07285 = 0.15459 -0.05401 -0.00716 -0.00662 C35 1 0.818889 0.663607 0.430876 11.00000 0.08099 0.08600 = 0.09654 -0.02700 -0.01538 -0.01026 AFIX 43 H35 2 0.843556 0.604652 0.469308 11.00000 -1.20000 AFIX 0 F8 5 0.956493 0.736075 0.569174 11.00000 0.41178 0.18583 = 0.10165 -0.03261 -0.04698 -0.01289 C38 1 0.814685 0.726837 0.547714 11.00000 0.15183 0.09408 = 0.10305 -0.02464 -0.07307 0.03118 PART 1 F10 5 0.750865 0.520494 0.365403 10.50000 0.14649 0.06553 = 0.23971 -0.08801 -0.00043 -0.01106 F11 5 0.958611 0.581753 0.285030 10.50000 0.06680 0.26615 = 0.48329 -0.32295 0.01727 0.00635 F12 5 0.717791 0.585228 0.266994 10.40000 0.14700 0.06769 = 0.23935 -0.08899 -0.00132 -0.01113 PART 2 F10' 5 0.885767 0.520809 0.359696 10.50000 0.53765 0.13454 = 0.19484 -0.08525 -0.00482 0.13891 F11' 5 0.876593 0.614784 0.237757 10.50000 0.21198 0.17755 = 0.19761 -0.09223 -0.00593 -0.01959 F12' 5 0.722533 0.617840 0.234996 10.60000 0.21342 0.17580 = 0.19737 -0.09421 -0.00844 -0.02292 PART 0 C39 1 0.826294 0.589725 0.319364 11.00000 0.11801 0.09063 = 0.12926 -0.05380 -0.01121 -0.01065 HKLF 4 REM mo_d8v18672_0m_a.res in P1 REM R1 = 0.1053 for 8305 Fo > 4sig(Fo) and 0.1529 for all 14162 data REM 1079 parameters refined using 186 restraints END WGHT 0.1878 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 x, y+1, z-1 HTAB N1 Br2_$1 HTAB N1 O3 HTAB N2 Br2_$1 EQIV $2 x, y-1, z+1 HTAB N3 Br1_$2 HTAB N3 O4 HTAB N4 Br1_$2 HTAB O4 Br1_$2 HTAB C1 Br1 HTAB C1 O3 HTAB C12 O1 HTAB C31 Br1 EQIV $3 x+1, y, z HTAB C31 O1_$3 HTAB C40 O4 HTAB C55 O2 HTAB C70 Br2_$3 HTAB C70 O2_$3 REM Highest difference peak 0.702, deepest hole -0.494, 1-sigma level 0.101 Q1 1 0.2043 -0.4612 1.0427 11.00000 0.05 0.70 Q2 1 1.2432 0.3960 0.7399 11.00000 0.05 0.59 Q3 1 0.6877 0.6869 0.5917 11.00000 0.05 0.54 Q4 1 0.4161 -0.4259 0.7349 11.00000 0.05 0.48 Q5 1 0.9375 0.6627 0.5981 11.00000 0.05 0.47 Q6 1 1.1101 0.3087 0.3822 11.00000 0.05 0.46 Q7 1 0.5784 0.3380 0.5218 11.00000 0.05 0.45 Q8 1 1.2023 0.4925 0.6213 11.00000 0.05 0.44 Q9 1 0.2355 0.0589 0.9419 11.00000 0.05 0.44 Q10 1 0.6593 0.3959 0.5257 11.00000 0.05 0.43 Q11 1 1.3676 0.3430 0.3992 11.00000 0.05 0.41 Q12 1 0.6806 0.4241 0.6215 11.00000 0.05 0.40 Q13 1 -0.4491 1.3627 0.2186 11.00000 0.05 0.37 Q14 1 0.0020 1.4387 -0.0989 11.00000 0.05 0.37 Q15 1 0.3092 0.9978 -0.0375 11.00000 0.05 0.35 Q16 1 1.2191 0.1823 0.6272 11.00000 0.05 0.35 Q17 1 0.5508 0.3010 0.6237 11.00000 0.05 0.35 Q18 1 -0.5386 1.4187 0.2443 11.00000 0.05 0.34 Q19 1 -0.1425 1.4596 0.2211 11.00000 0.05 0.34 Q20 1 0.2097 -0.2434 0.6835 11.00000 0.05 0.34 ; _shelx_res_checksum 6882 _shelx_hkl_file ; -1 0 0 22.10 4.60 2 0 0 1125.49 201.28 -3 0 0 642.34 115.79 -4 0 0 1830.52 327.77 5 0 0 593.64 107.99 6 0 0 455.15 83.89 7 0 0 6.40 7.20 7 0 0 0.20 7.40 8 0 0 16.50 10.60 8 0 0 20.20 9.90 9 0 0 4.70 12.10 10 0 0 14.70 13.30 11 0 0 22.20 12.40 11 -1 0 3.50 11.70 10 -1 0 2.20 11.70 9 -1 0 0.10 10.10 8 -1 0 -11.40 6.70 8 -1 0 -1.60 7.70 7 -1 0 32.70 12.90 7 -1 0 76.89 16.00 6 -1 0 189.78 31.00 6 -1 0 119.99 29.10 5 -1 0 239.48 42.20 5 -1 0 203.58 42.20 4 -1 0 750.82 118.49 -4 1 0 634.74 116.59 -4 1 0 618.04 116.59 -3 1 0 3261.17 565.74 -3 1 0 3093.39 565.74 1 -1 0 820.92 138.69 -1 1 0 777.12 138.69 -1 1 0 736.33 138.69 0 1 0 -0.20 0.20 1 1 0 310.67 54.79 1 1 0 300.57 54.99 -2 -1 0 2657.33 445.26 -2 -1 0 2442.56 445.26 2 1 0 2629.84 445.96 2 1 0 2281.47 445.16 -3 -1 0 937.91 158.98 -3 -1 0 829.82 159.98 -4 -1 0 2806.62 512.65 -4 -1 0 3013.80 514.45 -4 -1 0 2831.12 512.75 -5 -1 0 30.80 6.10 -5 -1 0 29.80 6.20 -5 -1 0 32.10 10.30 5 1 0 41.20 10.10 -6 -1 0 439.86 80.89 -6 -1 0 370.16 83.29 -6 -1 0 484.65 80.89 6 1 0 495.95 83.79 7 1 0 5.70 7.90 7 1 0 2.50 7.20 8 1 0 3.00 8.20 8 1 0 6.30 8.20 9 1 0 17.10 13.70 10 1 0 37.70 16.40 11 1 0 3.50 11.90 11 -2 0 3.50 11.50 10 -2 0 -6.60 11.90 9 -2 0 -8.50 9.70 8 -2 0 6.30 9.00 7 -2 0 5.00 8.70 7 -2 0 12.00 8.20 6 -2 0 202.98 33.10 6 -2 0 145.99 31.50 -6 2 0 145.59 28.90 -6 2 0 170.68 29.00 -5 2 0 209.18 38.00 -5 2 0 211.08 38.00 -4 2 0 663.03 117.19 -4 2 0 648.34 117.19 3 -2 0 920.11 166.68 -3 2 0 834.52 166.88 -3 2 0 1054.09 166.98 2 -2 0 85.09 15.10 2 -2 0 97.99 15.20 -2 2 0 79.09 15.20 -2 2 0 66.99 15.20 0 -2 0 32.90 6.40 0 2 0 35.00 6.40 0 2 0 27.70 5.90 -1 -2 0 2780.32 533.55 1 2 0 3209.78 533.65 -3 -2 0 2860.71 489.75 3 2 0 2636.24 489.55 -4 -2 0 465.65 83.29 -4 -2 0 405.46 84.49 -4 -2 0 470.05 83.29 4 2 0 493.45 82.89 4 2 0 460.85 82.79 -5 -2 0 423.16 80.19 -5 -2 0 536.95 82.69 -5 -2 0 428.16 80.19 -6 -2 0 348.87 61.09 -6 -2 0 360.36 58.09 -6 -2 0 302.97 57.99 6 2 0 264.17 60.19 -7 -2 0 96.69 22.70 -7 -2 0 90.59 17.70 -7 -2 0 92.79 17.60 7 2 0 116.69 23.00 -8 -2 0 54.99 11.30 8 2 0 84.79 18.20 8 2 0 81.19 19.00 9 2 0 13.70 10.50 10 2 0 4.40 10.70 11 2 0 -10.60 11.60 11 -3 0 -16.50 10.90 10 -3 0 0.50 11.60 9 -3 0 -7.70 7.90 9 -3 0 8.70 10.80 8 -3 0 16.90 11.10 7 -3 0 13.20 7.90 7 -3 0 7.30 8.00 -7 3 0 2.10 2.40 -7 3 0 7.30 3.00 6 -3 0 237.58 44.30 -6 3 0 238.18 42.00 -6 3 0 221.38 41.90 5 -3 0 194.68 39.40 5 -3 0 215.18 39.50 -5 3 0 208.58 37.60 -5 3 0 204.28 37.60 4 -3 0 114.09 25.80 4 -3 0 145.29 26.10 4 -3 0 155.18 23.90 4 -3 0 117.09 23.80 -4 3 0 123.39 25.60 3 -3 0 340.47 57.99 -3 3 0 327.37 58.79 -3 3 0 262.67 58.09 -3 3 0 364.36 58.29 2 -3 0 1355.76 217.68 2 -3 0 1177.98 217.58 -2 3 0 1168.98 217.68 -2 3 0 1173.28 217.68 1 -3 0 3956.70 773.82 1 -3 0 4632.84 773.52 -1 3 0 4435.46 773.62 0 -3 0 893.81 172.38 0 -3 0 1070.89 172.78 0 3 0 940.51 172.78 1 3 0 4439.46 917.21 1 3 0 5872.61 917.61 -2 -3 0 79.99 15.20 2 3 0 66.29 14.40 2 3 0 86.59 15.20 -3 -3 0 1634.94 309.47 3 3 0 1815.62 309.47 3 3 0 1751.42 309.37 -4 -3 0 157.28 27.60 -4 -3 0 164.58 27.80 4 3 0 122.09 27.20 4 3 0 175.78 27.50 4 3 0 121.09 28.50 -5 -3 0 136.59 32.80 -5 -3 0 174.28 31.30 -5 -3 0 152.38 31.10 5 3 0 245.28 34.10 -6 -3 0 335.07 58.89 -6 -3 0 291.07 58.79 6 3 0 381.86 61.59 -7 -3 0 164.98 31.60 -7 -3 0 165.68 35.70 -7 -3 0 173.08 31.60 7 3 0 190.78 35.20 -8 -3 0 15.20 10.20 -8 -3 0 -2.00 2.40 -8 -3 0 6.80 3.10 8 3 0 -11.00 6.90 9 3 0 23.30 13.00 10 3 0 14.00 12.40 11 3 0 -8.10 11.70 10 -4 0 11.00 12.30 9 -4 0 6.20 9.50 9 -4 0 3.90 10.60 8 -4 0 22.60 11.80 -8 4 0 20.40 5.10 7 -4 0 11.40 7.80 7 -4 0 9.10 8.90 -7 4 0 13.40 4.00 -7 4 0 8.40 4.10 6 -4 0 168.28 26.10 6 -4 0 111.89 24.80 -6 4 0 105.89 22.40 5 -4 0 18.90 8.20 5 -4 0 45.60 11.40 -5 4 0 24.80 6.20 -5 4 0 23.20 6.40 4 -4 0 161.68 28.90 4 -4 0 125.69 27.20 4 -4 0 143.49 27.20 -4 4 0 156.38 27.80 -4 4 0 186.58 28.90 3 -4 0 140.79 29.60 3 -4 0 173.78 29.00 -3 4 0 172.38 29.40 -3 4 0 135.69 29.50 -3 4 0 157.48 29.30 2 -4 0 1780.72 301.07 -2 4 0 1635.14 301.07 -2 4 0 1642.04 301.17 1 -4 0 357.66 69.39 1 -4 0 399.76 68.99 1 -4 0 325.87 69.39 -1 4 0 417.16 69.69 -1 4 0 427.96 69.69 0 -4 0 856.21 159.48 0 -4 0 793.32 159.08 0 -4 0 1021.10 159.68 0 4 0 864.61 159.58 0 4 0 932.11 159.68 -1 -4 0 911.31 143.99 -1 -4 0 769.42 143.89 1 4 0 675.23 143.69 1 4 0 860.41 143.99 2 4 0 1371.46 245.28 -3 -4 0 163.68 35.50 -3 -4 0 189.58 34.90 3 4 0 228.38 35.20 3 4 0 169.28 35.30 -4 -4 0 649.04 92.59 4 4 0 421.86 91.19 4 4 0 438.16 90.39 4 4 0 545.25 90.59 -5 -4 0 83.69 16.40 -5 -4 0 62.39 12.80 -5 -4 0 60.99 12.80 5 4 0 61.09 15.00 5 4 0 54.59 12.40 -6 -4 0 173.18 39.60 -6 -4 0 203.58 39.70 -6 -4 0 201.18 42.10 6 4 0 225.88 38.90 6 4 0 242.98 39.00 6 4 0 225.68 42.10 -7 -4 0 106.49 20.40 -7 -4 0 75.89 17.00 -7 -4 0 103.89 22.60 7 4 0 88.49 21.50 -8 -4 0 21.90 12.00 -8 -4 0 18.10 6.30 -8 -4 0 18.30 5.90 -9 -4 0 5.50 11.60 -9 -4 0 6.20 4.10 -9 -4 0 3.30 3.80 9 4 0 22.70 12.30 -10 -4 0 11.10 4.00 10 4 0 10.10 11.90 11 4 0 11.50 12.40 10 -5 0 -10.30 10.30 9 -5 0 -0.80 10.50 -9 5 0 -1.70 2.80 8 -5 0 16.20 10.00 8 -5 0 19.40 11.40 -8 5 0 19.80 5.40 -8 5 0 11.90 5.40 7 -5 0 32.70 12.30 7 -5 0 58.59 14.40 -7 5 0 52.99 10.50 -7 5 0 35.60 9.50 6 -5 0 18.80 8.50 6 -5 0 17.20 9.40 -6 5 0 14.50 5.50 -6 5 0 16.30 5.80 5 -5 0 9.10 3.30 5 -5 0 18.60 7.90 -5 5 0 12.90 4.90 -5 5 0 8.90 6.00 -5 5 0 8.40 4.30 4 -5 0 163.18 33.70 4 -5 0 177.98 33.80 4 -5 0 215.18 35.10 -4 5 0 208.08 35.00 -4 5 0 144.29 34.00 -4 5 0 223.58 34.60 3 -5 0 1011.60 198.98 3 -5 0 1102.29 199.08 3 -5 0 1296.57 199.28 -3 5 0 1045.20 199.28 2 -5 0 170.58 27.10 2 -5 0 155.38 26.30 -2 5 0 106.49 26.00 1 -5 0 84.79 17.40 1 -5 0 89.79 18.20 -1 5 0 120.19 18.00 -1 5 0 82.39 18.20 0 -5 0 118.09 28.80 0 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433.96 72.69 3 -7 0 423.66 72.79 -3 7 0 345.87 72.79 -3 7 0 384.36 72.79 2 -7 0 18.70 9.30 2 -7 0 32.10 7.70 2 -7 0 28.00 6.70 -2 7 0 23.50 7.90 -2 7 0 32.70 7.90 -2 7 0 14.40 7.40 1 -7 0 152.88 33.70 1 -7 0 185.58 33.10 -1 7 0 176.78 34.10 -1 7 0 201.48 34.60 0 -7 0 40.80 10.10 0 -7 0 34.70 8.70 0 -7 0 17.10 8.40 0 7 0 38.00 9.80 0 7 0 38.50 9.90 0 7 0 50.49 8.80 -1 -7 0 150.98 38.20 -1 -7 0 210.28 38.40 1 7 0 240.18 38.20 1 7 0 235.48 39.30 1 7 0 195.38 38.60 -2 -7 0 145.19 28.10 -2 -7 0 133.09 28.00 2 7 0 144.39 27.70 2 7 0 158.28 29.50 -3 -7 0 283.37 50.19 -3 -7 0 304.67 50.49 3 7 0 260.37 50.19 3 7 0 232.78 49.99 -4 -7 0 123.29 21.80 4 7 0 121.49 21.90 4 7 0 102.59 21.20 4 7 0 74.79 21.60 -5 -7 0 39.00 11.50 -5 -7 0 19.70 7.90 -5 -7 0 35.10 8.60 5 7 0 18.70 6.60 5 7 0 27.20 8.00 5 7 0 10.00 7.80 -6 -7 0 34.20 9.50 -6 -7 0 75.59 15.70 -6 -7 0 20.60 8.60 6 7 0 19.10 10.50 6 7 0 35.30 8.90 6 7 0 26.60 8.30 -7 -7 0 21.80 8.00 -7 -7 0 16.90 11.30 -7 -7 0 26.40 8.00 7 7 0 22.60 7.00 -8 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348.67 70.99 0 8 0 434.86 70.99 0 8 0 367.66 71.89 -1 -8 0 71.29 18.60 -1 -8 0 93.99 18.80 1 8 0 78.39 17.30 1 8 0 102.99 19.40 1 8 0 100.09 19.60 -2 -8 0 18.00 6.40 -2 -8 0 5.20 5.80 -2 -8 0 10.60 5.70 2 8 0 6.70 5.10 2 8 0 10.70 5.60 2 8 0 1.00 5.30 -3 -8 0 282.07 57.39 3 8 0 293.97 57.49 3 8 0 359.36 57.99 3 8 0 303.07 57.19 -4 -8 0 116.79 20.90 -4 -8 0 66.39 17.70 -4 -8 0 103.39 17.80 4 8 0 68.29 17.50 4 8 0 56.39 17.30 4 8 0 86.29 18.40 -5 -8 0 57.19 13.20 -5 -8 0 54.69 13.40 -5 -8 0 45.20 14.70 5 8 0 65.99 14.80 5 8 0 34.60 11.80 -6 -8 0 40.10 14.30 -6 -8 0 33.10 10.40 -6 -8 0 39.10 10.80 6 8 0 42.80 10.90 6 8 0 34.30 11.90 6 8 0 33.90 9.60 -7 -8 0 22.30 8.40 -7 -8 0 18.30 12.20 -7 -8 0 29.30 9.00 7 8 0 26.90 8.10 -8 -8 0 7.10 5.70 -8 -8 0 4.90 10.60 -8 -8 0 9.60 6.00 8 8 0 2.20 4.50 -9 -8 0 0.60 10.90 -9 -8 0 0.40 5.70 -9 -8 0 -9.00 4.20 -10 -8 0 3.10 6.60 -10 -8 0 -12.20 11.30 -10 -8 0 5.50 6.20 9 -9 0 6.50 10.10 -9 9 0 7.50 6.40 -9 9 0 -1.40 5.50 8 -9 0 7.00 8.40 8 -9 0 7.50 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150.38 33.30 -3 -9 0 214.98 34.50 -3 -9 0 192.98 34.80 3 9 0 120.39 33.10 3 9 0 207.38 34.70 -4 -9 0 86.89 17.90 -4 -9 0 98.49 19.60 -4 -9 0 94.09 18.20 4 9 0 72.19 16.90 4 9 0 46.60 16.50 4 9 0 60.89 16.60 -5 -9 0 80.29 26.80 -5 -9 0 154.28 26.90 5 9 0 115.29 26.30 5 9 0 117.79 25.70 5 9 0 169.78 27.30 -6 -9 0 34.60 12.00 -6 -9 0 62.99 13.70 -6 -9 0 47.40 15.50 6 9 0 48.70 12.60 -7 -9 0 5.20 10.40 -7 -9 0 13.50 7.20 -7 -9 0 4.50 5.80 7 9 0 -3.10 6.20 -8 -9 0 5.60 11.30 -8 -9 0 19.10 7.50 -8 -9 0 3.60 6.30 8 9 0 2.60 5.20 -9 -9 0 11.70 6.60 -9 -9 0 5.90 6.90 -9 -9 0 25.10 13.00 -10 -9 0 4.80 5.90 -10 -9 0 0.90 6.40 -10 -9 0 3.60 10.30 -9 10 0 9.30 7.00 -9 10 0 0.40 6.30 8 -10 0 19.70 9.30 8 -10 0 12.00 8.90 -8 10 0 8.70 7.10 -8 10 0 -1.60 6.70 7 -10 0 2.90 7.70 -7 10 0 13.90 7.50 -7 10 0 30.90 9.40 -7 10 0 -1.80 6.80 6 -10 0 10.00 7.40 6 -10 0 11.10 5.80 -6 10 0 6.60 7.20 -6 10 0 13.80 8.10 -6 10 0 14.60 7.30 5 -10 0 -1.30 5.00 5 -10 0 7.10 5.80 -5 10 0 15.60 7.30 -5 10 0 5.50 6.70 -5 10 0 10.30 7.90 4 -10 0 2.90 5.90 4 -10 0 8.60 5.30 4 -10 0 10.10 5.90 -4 10 0 6.80 7.30 -4 10 0 4.70 6.20 -4 10 0 7.80 6.90 3 -10 0 -3.20 4.50 3 -10 0 -5.80 4.00 3 -10 0 3.80 5.20 -3 10 0 4.30 5.60 -3 10 0 -5.90 5.90 -3 10 0 -0.70 6.50 2 -10 0 6.90 5.70 2 -10 0 6.60 5.30 2 -10 0 10.30 6.50 -2 10 0 1.50 7.10 -2 10 0 5.90 6.00 -2 10 0 10.60 6.80 1 -10 0 181.18 32.50 1 -10 0 141.99 32.00 1 -10 0 167.68 31.10 -1 10 0 164.48 31.50 -1 10 0 154.18 33.10 0 -10 0 7.00 5.30 0 -10 0 8.20 6.30 0 -10 0 6.70 6.90 0 10 0 8.10 5.30 0 10 0 4.70 12.20 0 10 0 4.60 6.30 -1 -10 0 370.96 61.29 -1 -10 0 260.97 60.09 1 10 0 280.47 60.79 1 10 0 335.17 59.79 1 10 0 416.06 62.39 -2 -10 0 16.70 7.80 -2 -10 0 20.50 8.70 -2 -10 0 15.20 8.70 2 10 0 22.70 7.40 2 10 0 11.30 7.60 2 10 0 14.40 8.40 -3 -10 0 34.00 11.60 -3 -10 0 63.79 14.40 -3 -10 0 51.59 12.80 3 10 0 37.10 12.70 3 10 0 35.80 11.10 3 10 0 30.70 11.20 -4 -10 0 21.50 9.50 -4 -10 0 53.29 13.70 -4 -10 0 37.80 10.70 4 10 0 16.30 9.50 4 10 0 19.20 10.30 4 10 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85.19 21.30 -2 11 0 101.89 22.20 -2 11 0 142.49 24.80 -2 11 0 59.09 19.80 1 -11 0 31.00 10.50 1 -11 0 38.70 11.90 1 -11 0 29.30 10.60 -1 11 0 54.99 12.00 -1 11 0 61.39 14.90 -1 11 0 28.50 11.50 0 -11 0 13.80 7.00 0 -11 0 -0.90 6.30 0 -11 0 2.80 5.50 0 11 0 11.10 5.70 0 11 0 1.70 7.00 0 11 0 27.20 10.70 -1 -11 0 127.29 24.20 -1 -11 0 161.48 24.90 1 11 0 74.09 23.90 1 11 0 86.09 23.80 1 11 0 110.69 22.10 -2 -11 0 8.60 7.70 -2 -11 0 9.30 7.70 -2 -11 0 6.00 7.60 2 11 0 10.80 8.60 2 11 0 16.40 9.10 2 11 0 19.70 7.50 -3 -11 0 15.40 8.70 -3 -11 0 30.80 11.20 -3 -11 0 3.30 7.30 3 11 0 23.10 8.70 3 11 0 24.00 9.60 3 11 0 10.40 8.00 -4 -11 0 11.80 8.60 -4 -11 0 8.70 7.60 -4 -11 0 -1.80 6.00 4 11 0 -1.40 5.90 4 11 0 -9.70 4.30 4 11 0 1.10 7.00 -5 -11 0 68.29 16.60 -5 -11 0 54.89 15.80 5 11 0 59.19 15.90 -6 -11 0 1.50 10.10 -6 -11 0 3.90 6.50 6 11 0 -5.20 6.40 -7 -11 0 1.50 7.00 -7 -11 0 8.00 12.40 -7 -11 0 6.30 7.20 7 11 0 10.50 7.50 -8 -11 0 3.50 7.70 -8 -11 0 18.10 13.10 -8 -11 0 -8.80 5.60 8 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13.40 -7 -7 3 5.10 6.40 6 7 -3 38.70 10.00 6 7 -3 26.10 8.40 6 7 -3 35.80 10.50 -6 -7 3 21.60 9.10 -6 -7 3 23.20 11.80 -6 -7 3 29.30 9.90 5 7 -3 13.50 7.30 5 7 -3 10.40 7.00 -5 -7 3 27.30 8.80 -5 -7 3 24.90 11.30 -5 -7 3 21.70 8.10 4 7 -3 186.38 38.80 4 7 -3 261.77 39.60 -4 -7 3 169.58 38.40 -4 -7 3 201.88 38.90 3 7 -3 281.37 47.10 3 7 -3 263.07 47.00 -3 -7 3 199.48 46.40 -3 -7 3 248.88 46.70 2 7 -3 60.09 14.50 2 7 -3 46.70 12.90 2 7 -3 35.40 13.00 -2 -7 3 50.29 14.10 -2 -7 3 90.49 14.60 -2 -7 3 94.89 15.90 1 7 -3 145.89 30.20 1 7 -3 180.78 30.80 -1 -7 3 135.39 29.90 -1 -7 3 155.58 29.60 0 7 -3 3.80 6.00 0 7 -3 0.20 4.30 0 7 -3 3.10 4.70 0 -7 3 5.70 5.30 0 -7 3 6.30 4.60 0 -7 3 11.50 6.40 -1 7 -3 3.80 5.70 -1 7 -3 -4.60 3.40 1 -7 3 4.90 4.90 1 -7 3 12.70 6.10 1 -7 3 14.80 5.20 -2 7 -3 163.78 35.40 -2 7 -3 236.48 36.50 -2 7 -3 147.69 35.20 2 -7 3 212.08 35.80 2 -7 3 138.99 35.00 2 -7 3 221.88 34.80 -3 7 -3 106.49 20.70 -3 7 -3 67.69 19.50 3 -7 3 118.69 19.90 3 -7 3 96.09 19.10 3 -7 3 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9.30 -4 -6 10 5.80 8.20 3 6 -10 113.49 24.80 3 6 -10 118.09 25.80 -3 -6 10 68.59 23.60 -3 -6 10 136.49 26.50 2 6 -10 34.50 12.80 2 6 -10 18.90 11.30 2 6 -10 39.70 11.80 -2 -6 10 18.30 11.90 -2 -6 10 52.99 12.60 -2 -6 10 29.60 11.60 1 6 -10 173.78 35.70 1 6 -10 183.18 36.30 -1 -6 10 138.29 35.50 -1 -6 10 135.29 35.10 -1 -6 10 203.58 34.00 0 6 -10 -0.40 8.70 0 6 -10 -17.50 6.30 0 6 -10 -0.70 7.60 0 -6 10 7.80 7.50 0 -6 10 21.40 9.70 0 -6 10 5.40 8.00 -1 6 -10 65.09 18.20 -1 6 -10 82.99 20.20 1 -6 10 104.59 18.00 1 -6 10 46.60 17.00 1 -6 10 43.80 16.80 -2 6 -10 127.59 34.80 -2 6 -10 201.28 35.80 2 -6 10 162.88 35.30 -3 6 -10 91.99 19.80 -3 6 -10 44.50 17.20 3 -6 10 63.79 18.10 3 -6 10 68.09 16.90 -4 6 -10 -3.80 7.40 -4 6 -10 1.30 9.10 4 -6 10 -3.30 10.00 4 -6 10 -0.20 6.80 -5 6 -10 3.90 8.90 5 -6 10 4.50 7.40 5 -6 10 7.90 11.80 -6 6 -10 8.30 8.10 -6 6 -10 1.50 8.60 6 -6 10 9.70 11.80 6 -6 10 1.30 6.90 -7 6 -10 3.20 7.70 7 -6 10 16.50 6.90 7 -6 10 -3.20 11.90 -8 6 -10 5.40 7.90 8 -6 10 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132.39 30.50 1 -5 10 169.78 28.50 -2 5 -10 36.50 14.70 -2 5 -10 59.39 16.20 2 -5 10 56.69 15.90 2 -5 10 59.09 14.30 -3 5 -10 80.99 19.00 -3 5 -10 67.99 18.20 3 -5 10 40.10 15.90 3 -5 10 101.89 19.80 -4 5 -10 10.90 6.90 4 -5 10 12.40 10.40 4 -5 10 -10.40 5.50 -5 5 -10 6.10 8.50 -5 5 -10 8.30 9.20 5 -5 10 10.50 12.20 5 -5 10 8.00 7.20 -6 5 -10 6.30 8.40 -6 5 -10 -9.80 5.40 6 -5 10 14.10 8.00 6 -5 10 8.10 11.60 -7 5 -10 1.80 7.80 -7 5 -10 3.90 7.50 7 -5 10 -4.80 5.80 7 -5 10 1.00 12.30 -8 5 -10 -3.90 9.80 -8 5 -10 5.90 7.60 8 -5 10 19.30 15.90 -9 -4 10 2.30 7.30 -9 -4 10 -10.10 8.70 -9 -4 10 11.10 6.60 8 4 -10 6.90 6.20 -8 -4 10 14.70 11.60 -8 -4 10 5.60 6.60 -8 -4 10 20.70 9.00 7 4 -10 7.70 6.90 -7 -4 10 2.00 6.40 -7 -4 10 2.50 7.70 -7 -4 10 -18.90 6.50 6 4 -10 -5.20 5.80 -6 -4 10 7.30 7.30 -6 -4 10 11.00 9.20 -6 -4 10 4.70 6.70 5 4 -10 33.90 9.80 5 4 -10 31.30 9.20 -5 -4 10 33.30 12.20 -5 -4 10 18.70 9.80 -5 -4 10 9.90 8.60 4 4 -10 66.49 19.20 4 4 -10 79.99 18.60 4 4 -10 79.29 17.30 -4 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4 -10 1.60 8.00 6 -4 10 -3.90 6.40 6 -4 10 1.70 13.10 -7 4 -10 33.00 11.30 -7 4 -10 20.50 9.50 7 -4 10 17.30 14.70 -8 4 -10 24.90 10.20 -8 4 -10 15.60 8.70 8 -4 10 4.80 17.20 -9 -3 10 5.60 6.40 -9 -3 10 10.00 10.60 8 3 -10 9.10 5.40 -8 -3 10 3.60 7.60 -8 -3 10 0.50 8.60 -8 -3 10 0.20 6.00 7 3 -10 -6.50 5.10 -7 -3 10 -3.70 5.10 -7 -3 10 11.80 8.80 -7 -3 10 4.90 7.50 6 3 -10 6.70 6.30 6 3 -10 -3.30 6.10 -6 -3 10 -3.60 6.60 -6 -3 10 6.90 8.40 -6 -3 10 0.00 6.10 5 3 -10 40.80 13.20 5 3 -10 41.10 12.50 -5 -3 10 67.89 15.30 -5 -3 10 47.40 13.70 4 3 -10 17.40 8.60 4 3 -10 13.80 11.60 4 3 -10 18.10 6.90 -4 -3 10 8.70 8.30 -4 -3 10 -0.80 6.70 -4 -3 10 6.10 7.70 3 3 -10 84.69 17.30 3 3 -10 86.79 15.80 3 3 -10 44.70 15.80 -3 -3 10 46.60 14.70 -3 -3 10 46.70 16.20 -3 -3 10 75.59 17.50 2 3 -10 96.59 17.00 2 3 -10 66.09 17.00 2 3 -10 38.10 16.00 -2 -3 10 58.29 15.10 -2 -3 10 76.09 18.00 -2 -3 10 71.19 17.80 1 3 -10 80.79 20.20 1 3 -10 106.39 22.10 1 3 -10 116.39 23.70 -1 -3 10 128.19 20.30 -1 -3 10 51.39 19.90 -1 -3 10 85.69 22.00 0 3 -10 8.80 8.10 0 3 -10 4.70 7.20 0 3 -10 1.10 7.10 0 -3 10 6.40 6.60 0 -3 10 -2.00 6.50 0 -3 10 5.70 7.30 -1 3 -10 193.28 31.30 -1 3 -10 106.99 29.60 -1 3 -10 149.29 31.10 1 -3 10 124.99 30.60 1 -3 10 175.28 31.50 -2 3 -10 70.19 19.70 -2 3 -10 76.89 20.80 -2 3 -10 97.69 20.80 2 -3 10 79.09 18.80 2 -3 10 80.49 19.10 -3 3 -10 244.08 45.70 3 -3 10 210.78 44.70 3 -3 10 237.58 45.10 -4 3 -10 64.09 17.70 -4 3 -10 54.29 17.80 4 -3 10 112.09 20.70 4 -3 10 80.39 18.30 4 -3 10 87.29 20.70 -5 3 -10 11.50 9.20 -5 3 -10 6.60 8.30 5 -3 10 25.40 9.10 5 -3 10 18.00 12.40 -6 3 -10 10.00 8.90 -6 3 -10 10.70 8.00 6 -3 10 37.70 15.00 -7 3 -10 17.80 9.30 -7 3 -10 6.50 7.80 7 -3 10 24.40 7.80 7 -3 10 20.40 14.80 -8 3 -10 5.80 6.90 -8 3 -10 -2.80 7.00 8 -3 10 10.70 15.70 -9 3 -10 -4.00 6.20 -9 3 -10 4.00 8.30 9 -3 10 -1.90 13.80 -9 -2 10 2.20 7.50 -9 -2 10 -0.50 9.80 -9 -2 10 0.70 5.10 -8 -2 10 -5.80 6.60 -8 -2 10 -2.60 8.60 -8 -2 10 -3.10 5.50 7 2 -10 2.30 5.70 7 2 -10 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23.50 13.20 3 4 20 14.80 12.50 -4 -4 -20 4.10 12.00 3 -5 -20 21.00 13.20 -3 5 20 39.80 11.00 -3 5 20 13.50 22.40 -3 5 20 52.59 21.80 2 -5 -20 25.10 12.20 2 -5 -20 -2.20 7.40 -2 5 20 42.30 18.00 -2 5 20 -2.50 13.70 -2 5 20 -6.70 6.10 1 -5 -20 25.00 13.40 -1 5 20 67.79 20.50 -1 5 20 32.20 11.00 -1 5 20 22.70 18.30 0 -5 -20 8.70 11.80 0 5 20 5.40 8.00 0 5 20 8.20 13.40 -1 -5 -20 47.40 19.00 1 5 20 35.40 19.30 1 5 20 35.80 13.00 -2 -5 -20 0.80 13.30 -2 -5 -20 0.10 11.90 2 5 20 7.50 10.10 2 5 20 26.10 13.70 -3 -5 -20 23.90 16.30 -3 -5 -20 37.70 15.60 3 5 20 28.30 15.40 3 5 20 9.90 12.90 -4 -5 -20 12.90 14.70 3 -6 -20 47.60 13.40 -3 6 20 13.40 7.50 -3 6 20 31.00 25.00 -3 6 20 -3.10 13.90 2 -6 -20 23.60 17.70 -2 6 20 65.29 21.70 -2 6 20 32.50 10.30 -2 6 20 26.30 18.00 1 -6 -20 6.40 9.80 1 -6 -20 0.50 8.40 -1 6 20 11.20 7.70 -1 6 20 6.70 17.70 -1 6 20 16.20 15.90 0 -6 -20 -16.00 11.10 0 6 20 12.20 13.10 -1 -6 -20 0.00 12.30 1 6 20 36.50 14.20 1 6 20 2.50 8.80 -2 -6 -20 -27.50 11.60 -2 -6 -20 10.60 13.60 2 6 20 5.10 9.90 2 6 20 -9.10 13.80 -3 -6 -20 -8.50 10.70 -3 -6 -20 -8.20 12.40 3 6 20 51.29 17.60 3 6 20 25.70 13.10 -4 -6 -20 -2.80 13.00 4 6 20 14.00 12.80 3 -7 -20 18.50 11.80 -3 7 20 -1.30 5.50 -3 7 20 -7.80 12.10 2 -7 -20 15.30 12.80 -2 7 20 22.10 16.10 -2 7 20 19.50 7.50 -2 7 20 43.80 19.50 -2 7 20 12.30 11.40 1 -7 -20 12.50 11.50 1 -7 -20 -17.60 7.10 -1 7 20 3.90 6.30 -1 7 20 9.10 17.20 -1 7 20 -21.40 12.30 -1 7 20 2.80 10.10 0 -7 -20 21.70 15.30 0 7 20 27.10 17.80 0 7 20 30.80 10.40 -1 -7 -20 20.50 14.50 1 7 20 17.10 16.20 1 7 20 6.60 8.80 -2 -7 -20 -12.40 12.50 -2 -7 -20 3.70 12.20 2 7 20 10.90 15.50 2 7 20 10.60 10.60 -3 -7 -20 3.90 11.50 -3 -7 -20 26.90 14.70 3 7 20 10.40 11.70 -4 -7 -20 17.00 12.80 4 7 20 4.10 14.30 -3 8 20 11.60 5.40 2 -8 -20 26.10 13.80 -2 8 20 -13.50 13.90 -2 8 20 -8.70 11.90 -2 8 20 13.40 9.10 -2 8 20 6.70 5.70 1 -8 -20 39.70 17.20 -1 8 20 34.00 11.80 -1 8 20 8.80 15.40 -1 8 20 27.40 20.10 -1 8 20 26.30 8.90 0 -8 -20 10.30 10.60 0 8 20 13.70 16.10 0 8 20 9.00 10.00 0 8 20 3.70 7.40 -1 -8 -20 22.60 14.70 1 8 20 27.90 17.20 1 8 20 30.50 12.30 -2 -8 -20 -11.80 14.10 -2 -8 -20 1.20 11.40 2 8 20 -2.60 9.80 2 8 20 22.90 16.30 -3 -8 -20 0.40 13.30 -3 -8 -20 32.70 19.20 3 8 20 7.00 12.20 3 8 20 28.50 15.40 -4 -8 -20 10.20 12.60 4 8 20 17.60 12.90 -3 9 20 11.70 13.20 2 -9 -20 8.50 11.60 -2 9 20 20.80 16.60 -2 9 20 -6.70 6.20 -2 9 20 2.30 14.10 1 -9 -20 10.60 13.50 -1 9 20 41.10 16.50 -1 9 20 39.20 21.30 -1 9 20 41.30 11.50 0 9 20 -13.20 9.30 0 9 20 0.90 6.10 0 9 20 8.40 12.80 -1 -9 -20 21.40 14.20 1 9 20 25.80 10.40 1 9 20 9.40 13.80 -2 -9 -20 16.10 15.30 -2 -9 -20 -3.70 14.30 2 9 20 -21.30 11.70 2 9 20 4.40 9.80 -3 -9 -20 13.40 14.30 -3 -9 -20 -14.90 12.50 3 9 20 -16.60 10.30 3 9 20 3.00 12.70 2 -10 -20 16.10 12.30 -2 10 20 6.40 4.00 1 -10 -20 -5.20 12.20 -1 10 20 14.80 13.50 -1 10 20 -4.20 4.70 -1 10 20 18.70 11.30 -1 10 20 -2.00 14.70 0 -10 -20 -5.70 11.40 0 10 20 28.20 10.30 0 10 20 -5.10 5.70 -1 -10 -20 14.80 13.50 1 10 20 22.90 18.30 1 10 20 17.10 10.10 1 10 20 4.30 12.60 -2 -10 -20 -9.60 10.60 2 10 20 -26.90 11.50 2 10 20 1.90 9.60 -3 -10 -20 10.90 13.20 -3 -10 -20 -15.50 15.00 3 10 20 -3.90 10.40 3 10 20 18.10 14.10 1 -11 -20 -4.70 11.40 -1 11 20 15.50 16.30 -1 11 20 1.50 14.80 -1 11 20 3.80 4.70 0 -11 -20 15.10 15.00 0 11 20 8.30 6.30 0 11 20 50.09 17.00 0 11 20 6.30 15.60 -1 -11 -20 -7.10 12.40 1 11 20 2.40 11.00 1 11 20 -10.50 7.90 1 11 20 22.80 15.80 -2 -11 -20 -7.20 11.80 2 11 20 -9.70 9.60 2 11 20 -2.40 13.40 0 -12 -20 4.50 12.50 0 12 20 -3.80 5.00 0 12 20 6.80 15.90 -1 -12 -20 -11.90 12.80 1 12 20 0.80 8.00 1 12 20 0.30 16.30 1 -3 -21 20.10 13.50 -1 3 21 9.70 15.70 -1 3 21 0.80 7.70 0 -3 -21 14.40 14.70 0 3 21 -4.50 8.00 0 3 21 -9.50 15.30 -1 -3 -21 4.50 12.10 1 3 21 -4.30 16.60 1 3 21 -5.30 8.50 -1 4 21 9.70 17.10 -1 4 21 15.80 9.40 0 -4 -21 10.60 13.80 0 4 21 5.90 7.80 0 4 21 -1.80 13.90 -1 -4 -21 -9.30 12.00 1 4 21 -18.70 13.10 1 4 21 30.50 10.30 1 -5 -21 11.50 12.40 -1 5 21 11.80 16.60 -1 5 21 2.70 7.90 0 -5 -21 -18.90 9.80 0 5 21 5.50 8.00 0 5 21 22.20 18.40 -1 -5 -21 18.60 14.80 1 5 21 12.30 14.90 1 5 21 14.50 9.60 -2 -5 -21 -0.20 13.10 2 5 21 -5.50 14.90 2 5 21 1.80 8.10 1 -6 -21 -7.20 12.90 -1 6 21 19.90 18.70 0 -6 -21 47.30 18.60 0 6 21 25.50 24.90 0 6 21 56.09 14.10 -1 -6 -21 11.00 13.40 1 6 21 -0.10 8.60 1 6 21 -13.20 13.70 -2 -6 -21 13.60 12.90 2 6 21 1.80 9.10 2 6 21 -20.40 10.10 1 -7 -21 -9.00 10.80 -1 7 21 2.00 6.70 -1 7 21 8.20 16.20 -1 7 21 9.60 14.00 0 -7 -21 41.90 19.60 0 7 21 42.40 12.70 -1 -7 -21 -4.60 15.10 1 7 21 14.10 14.80 1 7 21 14.80 9.40 -2 -7 -21 32.10 16.10 2 7 21 10.30 15.10 2 7 21 8.60 10.20 1 -8 -21 17.80 12.60 -1 8 21 13.80 16.00 -1 8 21 2.80 6.80 0 -8 -21 14.10 14.00 0 8 21 20.90 18.20 0 8 21 18.30 9.20 -1 -8 -21 17.20 23.40 1 8 21 -3.10 8.30 1 8 21 30.80 18.40 -2 -8 -21 3.90 12.60 2 8 21 18.50 11.60 2 8 21 24.30 17.70 0 -9 -21 -6.40 13.00 0 9 21 23.70 8.20 0 9 21 -6.30 18.00 1 9 21 32.20 20.70 1 9 21 20.10 10.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1574 loop_ _space_group_symop_operation_xyz 'x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.6983(2) 0.8807(2) 0.04967(13) 0.1335(10) Uani 1 1 d . . . . . Br2 Br 0.1752(3) 0.1145(2) 0.92281(15) 0.1409(11) Uani 1 1 d . . . . . P1 P 0.5063(4) 0.9765(2) 0.2556(2) 0.0575(8) Uani 1 1 d . . . . . P2 P 0.9796(3) 0.0260(2) 0.71818(19) 0.0530(7) Uani 1 1 d . . . . . N1 N 0.1667(12) 0.9931(8) 0.1580(7) 0.064(3) Uani 1 1 d . . . . . H1 H 0.1949 1.0013 0.1060 0.076 Uiso 1 1 calc R U . . . N2 N 0.0275(15) 1.1321(8) 0.1059(7) 0.076(3) Uani 1 1 d . . . . . H2 H 0.0607 1.1275 0.0577 0.091 Uiso 1 1 calc R U . . . N3 N 0.6495(13) -0.0029(7) 0.8199(7) 0.062(3) Uani 1 1 d . . . . . H3 H 0.6897 -0.0166 0.8700 0.074 Uiso 1 1 calc R U . . . N4 N 0.5461(15) -0.1392(8) 0.8710(7) 0.073(3) Uani 1 1 d . . . . . H4 H 0.5829 -0.1382 0.9187 0.088 Uiso 1 1 calc R U . . . O1 O 0.0224(11) 1.0500(6) 0.2484(5) 0.068(2) Uani 1 1 d . . . . . O2 O 0.5124(11) -0.0530(6) 0.7306(6) 0.067(2) Uani 1 1 d . . . . . O3 O 0.330(3) 0.9202(18) 0.0178(13) 0.202(10) Uani 1 1 d G . . . . H3C H 0.3399 0.8624 0.0453 0.304 Uiso 1 1 d G U . . . H3D H 0.3139 0.9225 -0.0336 0.304 Uiso 1 1 d G U . . . O4 O 0.822(4) 0.074(2) 0.9566(12) 0.226(13) Uani 1 1 d G . . . . H4A H 0.8332 0.0337 1.0055 0.339 Uiso 1 1 d G U . . . H4B H 0.7411 0.1084 0.9608 0.339 Uiso 1 1 d G U . . . C1 C 0.4037(12) 0.8969(8) 0.2216(8) 0.054(3) Uani 1 1 d . . . . . H1A H 0.4325 0.9019 0.1633 0.065 Uiso 1 1 calc R U . . . H1B H 0.4382 0.8342 0.2566 0.065 Uiso 1 1 calc R U . . . C2 C 0.2294(14) 0.9089(9) 0.2248(8) 0.058(3) Uani 1 1 d . . . . . H2A H 0.2006 0.9162 0.2804 0.070 Uiso 1 1 calc R U . . . C3 C 0.1626(16) 0.8228(11) 0.2177(11) 0.075(4) Uani 1 1 d . . . . . H3A H 0.0517 0.8322 0.2187 0.090 Uiso 1 1 calc R U . . . H3B H 0.1918 0.8134 0.1636 0.090 Uiso 1 1 calc R U . . . C4 C 0.2178(18) 0.7375(11) 0.2895(14) 0.090(5) Uani 1 1 d . U . . . C5 C 0.316(3) 0.6652(15) 0.2840(18) 0.124(7) Uani 1 1 d . U . . . H5 H 0.3573 0.6690 0.2307 0.149 Uiso 1 1 calc R U . . . C6 C 0.360(4) 0.585(2) 0.352(3) 0.153(9) Uani 1 1 d . U . . . H6 H 0.4090 0.5318 0.3421 0.183 Uiso 1 1 calc R U . . . C7 C 0.331(3) 0.5884(18) 0.425(2) 0.136(8) Uani 1 1 d . U . . . H7 H 0.3794 0.5421 0.4708 0.164 Uiso 1 1 calc R U . . . C8 C 0.227(3) 0.6584(18) 0.445(2) 0.149(11) Uani 1 1 d . . . . . H8 H 0.1995 0.6561 0.5003 0.178 Uiso 1 1 calc R U . . . C9 C 0.173(2) 0.7305(12) 0.3722(13) 0.096(5) Uani 1 1 d . . . . . H9 H 0.1021 0.7768 0.3800 0.116 Uiso 1 1 calc R U . . . C10 C 0.0673(15) 1.0572(9) 0.1753(8) 0.061(3) Uani 1 1 d . . . . . C11 C -0.0601(17) 1.2153(10) 0.1023(8) 0.067(3) Uani 1 1 d . . . . . C12 C -0.1300(19) 1.2302(10) 0.1751(10) 0.080(4) Uani 1 1 d . . . . . H12 H -0.1214 1.1841 0.2278 0.096 Uiso 1 1 calc R U . . . C13 C -0.2137(19) 1.3170(11) 0.1660(11) 0.085(4) Uani 1 1 d D . . . . C14 C -0.225(3) 1.3858(11) 0.0894(11) 0.100(6) Uani 1 1 d D . . . . H14 H -0.2832 1.4420 0.0845 0.120 Uiso 1 1 calc R U . A 1 C15 C -0.150(3) 1.3717(12) 0.0187(12) 0.111(6) Uani 1 1 d D U . . . C16 C -0.068(2) 1.2852(11) 0.0257(11) 0.090(5) Uani 1 1 d . . . . . H16 H -0.0200 1.2753 -0.0218 0.108 Uiso 1 1 calc R U . . . C17 C -0.297(3) 1.3287(14) 0.2422(12) 0.106(7) Uani 1 1 d D . . . . C19 C 0.4625(16) 0.9695(10) 0.3637(9) 0.068(3) Uani 1 1 d . . . . . C20 C 0.4061(18) 0.8908(11) 0.4173(9) 0.076(4) Uani 1 1 d . . . . . H20 H 0.3744 0.8473 0.3936 0.091 Uiso 1 1 calc R U . . . C21 C 0.395(2) 0.8737(17) 0.5027(11) 0.105(6) Uani 1 1 d . . . . . H21 H 0.3582 0.8192 0.5372 0.127 Uiso 1 1 calc R U . . . C22 C 0.438(3) 0.9396(19) 0.5370(12) 0.110(7) Uani 1 1 d . . . . . H22 H 0.4289 0.9303 0.5953 0.132 Uiso 1 1 calc R U . . . C23 C 0.494(2) 1.017(2) 0.4871(15) 0.124(9) Uani 1 1 d . . . . . H23 H 0.5234 1.0603 0.5120 0.148 Uiso 1 1 calc R U . . . C24 C 0.5104(19) 1.0348(13) 0.3993(11) 0.085(4) Uani 1 1 d . . . . . H24 H 0.5514 1.0881 0.3656 0.102 Uiso 1 1 calc R U . . . C25 C 0.4707(17) 1.0914(9) 0.1866(9) 0.069(3) Uani 1 1 d . . . . . C26 C 0.367(2) 1.1568(12) 0.2056(15) 0.099(5) Uani 1 1 d . . . . . H26 H 0.3147 1.1416 0.2571 0.118 Uiso 1 1 calc R U . . . C27 C 0.340(3) 1.2468(15) 0.146(2) 0.128(9) Uani 1 1 d . . . . . H27 H 0.2762 1.2929 0.1593 0.154 Uiso 1 1 calc R U . . . C28 C 0.410(4) 1.2651(16) 0.068(3) 0.156(14) Uani 1 1 d . . . . . H28 H 0.3851 1.3227 0.0279 0.188 Uiso 1 1 calc R U . . . C29 C 0.512(5) 1.2042(16) 0.0483(15) 0.154(13) Uani 1 1 d . . . . . H29 H 0.5600 1.2203 -0.0044 0.185 Uiso 1 1 calc R U . . . C30 C 0.545(3) 1.1167(14) 0.1069(12) 0.103(5) Uani 1 1 d . . . . . H30 H 0.6176 1.0742 0.0938 0.124 Uiso 1 1 calc R U . . . C31 C 0.7068(14) 0.9377(10) 0.2562(9) 0.066(3) Uani 1 1 d . . . . . H31A H 0.7365 0.9386 0.1989 0.079 Uiso 1 1 calc R U . . . H31B H 0.7655 0.9808 0.2724 0.079 Uiso 1 1 calc R U . . . C32 C 0.7465(15) 0.8404(10) 0.3171(10) 0.066(3) Uani 1 1 d . . . . . C33 C 0.7614(15) 0.7644(10) 0.2867(11) 0.072(4) Uani 1 1 d . . . . . H33 H 0.7463 0.7718 0.2291 0.087 Uiso 1 1 calc R U . . . C37 C 0.7690(17) 0.8278(10) 0.4028(10) 0.074(4) Uani 1 1 d . . . . . H37 H 0.7626 0.8791 0.4228 0.089 Uiso 1 1 calc R U . . . C36 C 0.8007(16) 0.7399(11) 0.4589(10) 0.079(4) Uani 1 1 d D . . . . C40 C 0.8473(13) 0.1028(9) 0.7548(8) 0.056(3) Uani 1 1 d . . . . . H40A H 0.8776 0.0988 0.8123 0.068 Uiso 1 1 calc R U . . . H40B H 0.8575 0.1660 0.7189 0.068 Uiso 1 1 calc R U . . . C41 C 0.6765(13) 0.0861(9) 0.7558(8) 0.056(3) Uani 1 1 d . . . . . H41 H 0.6492 0.0825 0.6995 0.067 Uiso 1 1 calc R U . . . C42 C 0.5775(15) 0.1680(10) 0.7712(12) 0.081(4) Uani 1 1 d . . . . . H42A H 0.4712 0.1548 0.7738 0.098 Uiso 1 1 calc R U . . . H42B H 0.6053 0.1728 0.8263 0.098 Uiso 1 1 calc R U . . . C43 C 0.5905(13) 0.2573(7) 0.7068(10) 0.096(6) Uani 1 1 d G . . . . C44 C 0.5633(14) 0.2693(9) 0.6209(10) 0.106(7) Uani 1 1 d G . . . . H44 H 0.5300 0.2210 0.6044 0.128 Uiso 1 1 calc R U . . . C45 C 0.5861(19) 0.3534(12) 0.5598(9) 0.137(8) Uani 1 1 d G U . . . H45 H 0.5679 0.3614 0.5023 0.165 Uiso 1 1 calc R U . . . C46 C 0.636(2) 0.4256(9) 0.5845(12) 0.147(9) Uani 1 1 d G U . . . H46 H 0.6512 0.4819 0.5436 0.176 Uiso 1 1 calc R U . . . C47 C 0.663(2) 0.4136(9) 0.6704(14) 0.182(13) Uani 1 1 d G U . . . H47 H 0.6966 0.4619 0.6869 0.219 Uiso 1 1 calc R U . . . C48 C 0.6404(19) 0.3295(10) 0.7315(10) 0.144(11) Uani 1 1 d G . . . . H48 H 0.6586 0.3214 0.7889 0.173 Uiso 1 1 calc R U . . . C49 C 0.5642(14) -0.0628(9) 0.8021(8) 0.059(3) Uani 1 1 d . . . . . C50 C 0.4759(16) -0.2180(10) 0.8736(9) 0.067(3) Uani 1 1 d . . . . . C51 C 0.4531(19) -0.2814(10) 0.9549(10) 0.077(4) Uani 1 1 d . . . . . H51 H 0.4849 -0.2691 1.0035 0.093 Uiso 1 1 calc R U . . . C52 C 0.386(2) -0.3589(10) 0.9626(12) 0.088(5) Uani 1 1 d . . . . . C53 C 0.338(2) -0.3818(11) 0.8925(14) 0.098(5) Uani 1 1 d . . . . . H53 H 0.2964 -0.4376 0.8991 0.117 Uiso 1 1 calc R U . . . C54 C 0.354(2) -0.3182(13) 0.8117(11) 0.089(5) Uani 1 1 d . . . . . C55 C 0.4237(19) -0.2381(10) 0.8029(10) 0.074(4) Uani 1 1 d . . . . . H55 H 0.4359 -0.1969 0.7486 0.089 Uiso 1 1 calc R U . . . C56 C 0.355(3) -0.4251(15) 1.0453(15) 0.116(7) Uani 1 1 d . . . . . C57 C 0.298(3) -0.3339(17) 0.7345(17) 0.117(7) Uani 1 1 d . . . . . C58 C 0.9817(16) -0.0900(9) 0.7863(9) 0.064(3) Uani 1 1 d . . . . . C59 C 1.051(2) -0.1118(11) 0.8667(11) 0.094(5) Uani 1 1 d . . . . . H59 H 1.1018 -0.0683 0.8823 0.113 Uiso 1 1 calc R U . . . C60 C 1.042(3) -0.1995(14) 0.9217(15) 0.109(6) Uani 1 1 d . . . . . H60 H 1.0955 -0.2146 0.9732 0.131 Uiso 1 1 calc R U . . . C61 C 0.972(3) -0.2597(15) 0.9100(18) 0.126(10) Uani 1 1 d . . . . . H61 H 0.9652 -0.3154 0.9534 0.151 Uiso 1 1 calc R U . . . C62 C 0.900(3) -0.2442(13) 0.830(2) 0.122(8) Uani 1 1 d . . . . . H62 H 0.8521 -0.2910 0.8183 0.146 Uiso 1 1 calc R U . . . C63 C 0.9034(19) -0.1538(10) 0.7662(13) 0.085(4) Uani 1 1 d . . . . . H63 H 0.8539 -0.1399 0.7136 0.102 Uiso 1 1 calc R U . . . C64 C 0.9374(14) 0.0341(10) 0.6089(8) 0.064(3) Uani 1 1 d . . . . . C65 C 1.0124(19) -0.0259(13) 0.5720(11) 0.083(4) Uani 1 1 d . . . . . H65 H 1.0746 -0.0773 0.6050 0.100 Uiso 1 1 calc R U . . . C66 C 0.996(3) -0.0100(19) 0.4830(16) 0.110(7) Uani 1 1 d . . . . . H66 H 1.0340 -0.0554 0.4587 0.132 Uiso 1 1 calc R U . . . C67 C 0.927(2) 0.067(2) 0.4360(14) 0.113(7) Uani 1 1 d . . . . . H67 H 0.9309 0.0806 0.3769 0.136 Uiso 1 1 calc R U . . . C68 C 0.852(2) 0.127(2) 0.4699(11) 0.126(8) Uani 1 1 d . . . . . H68 H 0.7936 0.1789 0.4347 0.152 Uiso 1 1 calc R U . . . C69 C 0.8583(17) 0.1134(11) 0.5592(9) 0.073(4) Uani 1 1 d . . . . . H69 H 0.8103 0.1571 0.5827 0.088 Uiso 1 1 calc R U . . . C70 C 1.1655(13) 0.0668(9) 0.7189(8) 0.058(3) Uani 1 1 d . . . . . H70A H 1.1896 0.0662 0.7763 0.070 Uiso 1 1 calc R U . . . H70B H 1.2419 0.0245 0.7030 0.070 Uiso 1 1 calc R U . . . C71 C 1.1737(14) 0.1646(9) 0.6580(9) 0.060(3) Uani 1 1 d . . . . . C72 C 1.2010(17) 0.1792(10) 0.5713(9) 0.072(3) Uani 1 1 d . . . . . H72 H 1.2201 0.1283 0.5512 0.086 Uiso 1 1 calc R U . . . C73 C 1.2000(19) 0.2674(10) 0.5155(9) 0.078(4) Uani 1 1 d D . . . . C74 C 1.1761(19) 0.3459(13) 0.5428(14) 0.094(5) Uani 1 1 d . . . . . H74 H 1.1786 0.4058 0.5051 0.113 Uiso 1 1 calc R U . . . C75 C 1.1487(16) 0.3302(10) 0.6280(12) 0.080(4) Uani 1 1 d D . . . . C76 C 1.1463(16) 0.2397(10) 0.6871(10) 0.073(4) Uani 1 1 d . . . . . H76 H 1.1266 0.2318 0.7445 0.087 Uiso 1 1 calc R U . . . C77 C 1.232(3) 0.2814(17) 0.4293(13) 0.123(8) Uani 1 1 d D . . . . C78 C 1.129(2) 0.4086(12) 0.6610(14) 0.107(6) Uani 1 1 d D U . . . F1 F -0.3547(16) 1.2570(10) 0.2917(9) 0.124(4) Uani 1 1 d . . . . . F2 F -0.191(2) 1.3424(14) 0.2991(10) 0.174(7) Uani 1 1 d . . . . . F3 F -0.390(3) 1.4039(12) 0.2269(9) 0.221(13) Uani 1 1 d . . . . . C18 C -0.149(3) 1.4455(18) -0.0639(17) 0.112(11) Uani 0.6 1 d D U P B 1 F4 F -0.253(6) 1.518(2) -0.0755(17) 0.18(2) Uani 0.5 1 d D . P B 1 F5 F -0.179(6) 1.418(2) -0.1311(17) 0.151(13) Uani 0.5 1 d D . P B 1 F6 F -0.018(5) 1.483(3) -0.080(3) 0.23(3) Uani 0.5 1 d D . P B 1 C18' C -0.204(5) 1.442(3) -0.0606(17) 0.167(9) Uani 0.4 1 d D U P B 2 F4' F -0.339(5) 1.439(3) -0.094(3) 0.181(10) Uani 0.5 1 d D U P B 2 F5' F -0.090(6) 1.441(4) -0.115(3) 0.168(10) Uani 0.5 1 d D U P B 2 F6' F -0.195(6) 1.524(3) -0.046(3) 0.169(10) Uani 0.5 1 d D U P B 2 F7 F 0.822(4) 0.6491(14) 0.6002(11) 0.232(8) Uani 1 1 d D U . . . F9 F 0.762(4) 0.7921(14) 0.5782(10) 0.223(8) Uani 1 1 d D U . . . F13 F 0.459(3) -0.4247(12) 1.1065(12) 0.198(6) Uani 1 1 d . U . . . F14 F 0.239(4) -0.3951(14) 1.0846(13) 0.210(7) Uani 1 1 d . U . . . F15 F 0.374(3) -0.5084(12) 1.0557(12) 0.198(6) Uani 1 1 d . U . . . F16 F 0.192(3) -0.3934(13) 0.7487(12) 0.177(5) Uani 1 1 d . U . . . F17 F 0.410(3) -0.3513(15) 0.6849(13) 0.186(5) Uani 1 1 d . U . . . F18 F 0.231(3) -0.2647(15) 0.6792(13) 0.172(5) Uani 1 1 d . U . . . F19 F 1.195(3) 0.2213(16) 0.3934(11) 0.208(7) Uani 1 1 d D U . . . F20 F 1.381(3) 0.2678(18) 0.4118(14) 0.233(7) Uani 1 1 d D U . . . F21 F 1.219(4) 0.3607(17) 0.3776(14) 0.236(8) Uani 1 1 d D U . . . F22 F 1.256(3) 0.4504(14) 0.660(2) 0.235(9) Uani 1 1 d D U . . . F23 F 1.047(3) 0.4829(14) 0.6071(19) 0.242(9) Uani 1 1 d D U . . . F24 F 1.057(4) 0.4025(10) 0.7286(14) 0.229(13) Uani 1 1 d D . . . . C34 C 0.8006(16) 0.6746(10) 0.3463(15) 0.089(5) Uani 1 1 d D . . . . C35 C 0.8189(19) 0.6636(12) 0.4309(13) 0.088(4) Uani 1 1 d . . . . . H35 H 0.8436 0.6047 0.4693 0.105 Uiso 1 1 calc R U . . . F8 F 0.956(4) 0.7361(16) 0.5692(12) 0.236(8) Uani 1 1 d D U . . . C38 C 0.815(3) 0.7268(13) 0.5477(12) 0.120(8) Uani 1 1 d D . . . . F10 F 0.751(4) 0.5205(17) 0.365(2) 0.141(10) Uani 0.5 1 d D U P C 1 F11 F 0.959(3) 0.582(4) 0.285(5) 0.23(3) Uani 0.5 1 d D . P C 1 F12 F 0.718(4) 0.585(2) 0.267(3) 0.142(10) Uani 0.4 1 d D U P C 1 F10' F 0.886(14) 0.521(4) 0.360(4) 0.29(5) Uani 0.5 1 d . . P C 2 F11' F 0.877(8) 0.615(3) 0.238(3) 0.188(12) Uani 0.5 1 d . U P C 2 F12' F 0.723(7) 0.618(3) 0.235(3) 0.187(12) Uani 0.6 1 d . U P C 2 C39 C 0.826(3) 0.5897(13) 0.3194(15) 0.108(6) Uani 1 1 d D 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 0.1117(15) 0.231(3) 0.0819(13) -0.0871(16) -0.0020(10) -0.0046(15) Br2 0.1464(19) 0.224(3) 0.0862(14) -0.0885(17) 0.0355(12) -0.0547(18) P1 0.0621(18) 0.0622(19) 0.0524(17) -0.0227(15) 0.0001(13) -0.0097(14) P2 0.0554(16) 0.0568(17) 0.0479(16) -0.0185(13) 0.0001(12) -0.0024(12) N1 0.062(6) 0.082(7) 0.046(5) -0.020(5) -0.002(4) 0.002(5) N2 0.092(8) 0.084(8) 0.046(6) -0.022(6) -0.001(5) 0.021(6) N3 0.077(7) 0.067(6) 0.045(5) -0.022(5) -0.001(5) -0.012(5) N4 0.105(9) 0.078(7) 0.043(6) -0.021(5) 0.003(5) -0.030(6) O1 0.082(6) 0.080(6) 0.041(4) -0.022(4) 0.011(4) 0.000(4) O2 0.079(6) 0.073(6) 0.050(5) -0.016(4) -0.005(4) -0.017(4) O3 0.21(2) 0.24(3) 0.143(18) -0.050(17) 0.021(16) 0.002(19) O4 0.25(3) 0.33(4) 0.098(14) -0.059(18) 0.002(15) -0.05(3) C1 0.049(6) 0.061(7) 0.057(7) -0.025(6) 0.000(5) 0.002(5) C2 0.058(6) 0.064(7) 0.055(7) -0.022(6) 0.003(5) -0.008(5) C3 0.058(7) 0.087(9) 0.089(10) -0.034(8) 0.007(7) -0.022(6) C4 0.068(7) 0.075(8) 0.126(11) -0.030(8) 0.004(8) -0.019(7) C5 0.114(11) 0.098(11) 0.146(13) -0.020(10) 0.027(10) -0.004(9) C6 0.147(14) 0.129(13) 0.175(16) -0.041(12) -0.002(12) 0.004(11) C7 0.120(12) 0.113(12) 0.153(14) -0.008(11) -0.009(11) -0.006(10) C8 0.102(15) 0.120(17) 0.17(3) 0.038(17) -0.004(15) -0.030(13) C9 0.086(11) 0.086(11) 0.102(14) -0.001(10) 0.014(9) -0.026(8) C10 0.066(7) 0.061(7) 0.056(8) -0.022(6) -0.003(5) 0.005(5) C11 0.084(9) 0.072(8) 0.045(7) -0.021(6) -0.007(6) 0.000(7) C12 0.098(10) 0.059(8) 0.070(9) -0.009(7) -0.004(8) 0.015(7) C13 0.093(10) 0.081(10) 0.091(12) -0.041(9) -0.006(8) 0.001(8) C14 0.148(16) 0.061(9) 0.076(11) -0.006(8) -0.008(10) 0.015(9) C15 0.165(19) 0.082(11) 0.088(11) -0.022(8) 0.037(11) -0.039(11) C16 0.122(13) 0.074(9) 0.060(9) -0.007(7) 0.013(8) 0.011(9) C17 0.147(17) 0.091(13) 0.077(12) -0.035(11) -0.008(12) 0.040(12) C19 0.073(8) 0.080(9) 0.055(7) -0.026(7) 0.001(6) 0.000(7) C20 0.086(9) 0.093(10) 0.052(8) -0.026(8) 0.001(7) -0.008(8) C21 0.095(12) 0.144(17) 0.052(9) 0.002(11) -0.003(8) 0.007(11) C22 0.116(14) 0.16(2) 0.049(9) -0.035(12) 0.013(10) 0.012(14) C23 0.088(12) 0.22(3) 0.087(14) -0.094(18) -0.021(11) 0.012(15) C24 0.085(10) 0.113(12) 0.080(10) -0.058(10) -0.003(8) -0.022(8) C25 0.079(8) 0.062(8) 0.067(8) -0.020(7) -0.017(7) -0.015(7) C26 0.101(12) 0.079(11) 0.119(15) -0.034(10) -0.027(10) -0.006(9) C27 0.131(18) 0.064(12) 0.17(3) -0.016(15) -0.055(18) 0.004(11) C28 0.20(3) 0.048(12) 0.19(4) 0.008(17) -0.06(3) -0.016(14) C29 0.30(4) 0.074(14) 0.075(14) 0.015(11) -0.052(18) -0.038(19) C30 0.137(16) 0.098(13) 0.071(11) -0.022(10) 0.002(10) -0.010(11) C31 0.060(7) 0.084(9) 0.057(8) -0.025(7) -0.002(6) -0.014(6) C32 0.054(7) 0.081(9) 0.073(9) -0.036(7) 0.004(6) -0.018(6) C33 0.061(7) 0.075(9) 0.093(11) -0.044(8) -0.003(7) -0.004(6) C37 0.074(8) 0.068(8) 0.080(10) -0.023(7) -0.012(7) -0.004(6) C36 0.060(7) 0.093(11) 0.087(11) -0.032(9) -0.012(7) -0.006(7) C40 0.050(6) 0.069(7) 0.056(7) -0.027(6) 0.005(5) -0.006(5) C41 0.049(6) 0.070(7) 0.046(6) -0.013(6) 0.002(5) -0.011(5) C42 0.045(6) 0.076(9) 0.115(13) -0.020(9) 0.010(7) -0.003(6) C43 0.049(7) 0.076(11) 0.145(18) -0.010(11) -0.002(9) 0.009(7) C44 0.062(9) 0.085(11) 0.147(19) -0.003(12) 0.002(10) 0.007(7) C45 0.111(11) 0.129(13) 0.144(14) -0.004(11) 0.002(10) -0.004(10) C46 0.136(13) 0.130(13) 0.156(15) -0.014(11) -0.004(11) -0.024(11) C47 0.174(17) 0.172(17) 0.204(18) -0.057(13) -0.009(13) -0.034(13) C48 0.139(19) 0.057(10) 0.23(3) -0.033(14) -0.042(19) -0.006(10) C49 0.061(7) 0.070(8) 0.048(7) -0.021(6) 0.010(5) -0.001(6) C50 0.072(8) 0.072(8) 0.061(8) -0.024(7) -0.001(6) -0.012(6) C51 0.097(10) 0.062(8) 0.066(9) -0.011(7) 0.000(7) -0.007(7) C52 0.110(12) 0.052(8) 0.090(12) -0.009(8) 0.007(9) -0.003(8) C53 0.131(14) 0.050(8) 0.111(15) -0.018(9) 0.022(11) -0.022(8) C54 0.111(12) 0.097(12) 0.069(10) -0.038(9) 0.003(8) -0.018(9) C55 0.099(10) 0.070(8) 0.065(8) -0.031(7) 0.009(7) -0.029(7) C56 0.16(2) 0.082(13) 0.083(14) 0.006(11) 0.002(14) -0.006(12) C57 0.17(2) 0.100(14) 0.113(17) -0.063(14) 0.044(16) -0.054(15) C58 0.074(8) 0.057(7) 0.061(8) -0.019(6) 0.005(6) -0.006(6) C59 0.131(14) 0.066(9) 0.072(10) -0.008(8) -0.017(10) 0.012(9) C60 0.143(17) 0.056(11) 0.110(16) 0.000(10) -0.002(12) -0.003(11) C61 0.15(2) 0.061(12) 0.115(19) 0.031(12) 0.043(16) 0.018(12) C62 0.133(17) 0.068(11) 0.16(2) -0.026(13) 0.047(17) -0.013(11) C63 0.089(10) 0.064(9) 0.107(13) -0.037(9) -0.001(9) 0.001(7) C64 0.059(7) 0.085(9) 0.056(7) -0.030(7) 0.007(6) -0.021(6) C65 0.087(10) 0.107(11) 0.071(9) -0.046(9) 0.018(7) -0.024(8) C66 0.105(14) 0.16(2) 0.112(16) -0.097(16) 0.032(13) -0.035(14) C67 0.084(12) 0.19(2) 0.075(12) -0.055(15) 0.006(10) -0.016(13) C68 0.096(13) 0.23(3) 0.051(9) -0.039(13) -0.001(9) -0.026(15) C69 0.075(8) 0.086(9) 0.054(8) -0.016(7) -0.011(6) 0.003(7) C70 0.054(6) 0.073(8) 0.051(7) -0.026(6) 0.006(5) -0.004(5) C71 0.052(6) 0.063(7) 0.064(8) -0.017(6) 0.006(5) -0.009(5) C72 0.081(9) 0.069(8) 0.068(9) -0.025(7) 0.010(7) -0.008(6) C73 0.092(10) 0.067(9) 0.072(9) -0.011(7) 0.017(7) -0.023(7) C74 0.072(9) 0.088(11) 0.123(16) -0.037(10) 0.015(9) -0.006(7) C75 0.063(8) 0.081(10) 0.108(13) -0.045(9) 0.013(8) -0.013(7) C76 0.065(8) 0.076(9) 0.077(10) -0.024(8) 0.017(7) -0.007(6) C77 0.116(16) 0.15(2) 0.103(16) -0.028(16) 0.045(13) -0.055(14) C78 0.097(10) 0.081(10) 0.146(13) -0.036(9) 0.019(9) -0.016(8) F1 0.138(9) 0.129(9) 0.105(8) -0.043(8) 0.028(7) 0.006(7) F2 0.220(18) 0.223(17) 0.116(11) -0.095(11) 0.023(11) -0.069(14) F3 0.36(3) 0.167(13) 0.082(8) -0.009(9) 0.019(12) 0.158(18) C18 0.128(16) 0.100(15) 0.106(15) -0.033(12) 0.029(12) 0.002(12) F4 0.33(6) 0.096(19) 0.075(16) 0.015(14) -0.05(2) 0.09(3) F5 0.24(4) 0.13(2) 0.076(15) -0.012(14) -0.02(2) -0.01(2) F6 0.29(6) 0.19(4) 0.16(3) 0.06(3) 0.00(3) -0.15(4) C18' 0.184(14) 0.143(12) 0.143(12) -0.003(9) -0.007(11) -0.006(11) F4' 0.201(17) 0.151(15) 0.152(15) 0.005(13) -0.015(15) -0.004(14) F5' 0.184(18) 0.145(15) 0.139(16) 0.003(14) 0.011(15) -0.003(15) F6' 0.193(17) 0.137(15) 0.149(16) -0.004(14) -0.011(15) -0.014(14) F7 0.42(3) 0.166(12) 0.094(8) -0.017(8) -0.037(11) -0.025(12) F9 0.41(3) 0.172(12) 0.088(7) -0.043(8) -0.056(11) 0.006(12) F13 0.314(17) 0.126(8) 0.112(8) 0.027(7) -0.020(10) -0.030(9) F14 0.308(18) 0.148(9) 0.116(9) 0.042(8) 0.000(11) -0.021(11) F15 0.325(18) 0.108(8) 0.129(9) 0.019(7) -0.019(10) -0.044(10) F16 0.230(13) 0.173(10) 0.156(11) -0.070(9) -0.014(10) -0.096(10) F17 0.233(14) 0.207(12) 0.152(11) -0.101(10) -0.002(10) -0.032(10) F18 0.225(12) 0.183(10) 0.137(9) -0.078(9) -0.021(9) -0.063(9) F19 0.33(2) 0.217(14) 0.103(9) -0.069(9) 0.073(12) -0.071(13) F20 0.33(2) 0.235(13) 0.125(9) -0.045(10) 0.086(12) -0.044(12) F21 0.35(2) 0.208(14) 0.124(10) -0.022(11) 0.081(13) -0.029(14) F22 0.259(19) 0.164(12) 0.34(2) -0.167(15) 0.055(18) -0.024(13) F23 0.269(19) 0.151(12) 0.34(3) -0.141(15) 0.056(18) 0.014(12) F24 0.40(3) 0.108(10) 0.207(19) -0.093(11) 0.16(2) -0.069(14) C34 0.053(7) 0.073(10) 0.155(18) -0.054(11) -0.007(9) -0.007(6) C35 0.081(10) 0.086(11) 0.097(12) -0.027(9) -0.015(9) -0.010(8) F8 0.41(2) 0.186(11) 0.102(7) -0.033(8) -0.047(11) -0.013(11) C38 0.152(19) 0.094(13) 0.103(16) -0.025(12) -0.073(14) 0.031(13) F10 0.146(17) 0.066(12) 0.24(3) -0.088(14) 0.00(2) -0.011(13) F11 0.067(13) 0.27(5) 0.48(8) -0.32(6) 0.02(3) 0.006(19) F12 0.147(17) 0.068(12) 0.24(3) -0.089(14) 0.00(2) -0.011(13) F10' 0.54(14) 0.13(3) 0.19(4) -0.09(3) 0.00(7) 0.14(6) F11' 0.212(18) 0.178(16) 0.198(16) -0.092(12) -0.006(13) -0.020(13) F12' 0.213(18) 0.176(17) 0.197(17) -0.094(13) -0.008(14) -0.023(14) C39 0.118(11) 0.091(10) 0.129(12) -0.054(9) -0.011(10) -0.011(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 C25 P1 C19 111.6(7) . . ? C25 P1 C1 111.5(6) . . ? C19 P1 C1 110.7(6) . . ? C25 P1 C31 110.1(7) . . ? C19 P1 C31 105.5(6) . . ? C1 P1 C31 107.2(6) . . ? C58 P2 C40 111.1(6) . . ? C58 P2 C70 109.9(6) . . ? C40 P2 C70 106.4(6) . . ? C58 P2 C64 111.4(6) . . ? C40 P2 C64 110.9(6) . . ? C70 P2 C64 106.9(6) . . ? C10 N1 C2 122.1(11) . . ? C10 N1 H1 119.0 . . ? C2 N1 H1 119.0 . . ? C10 N2 C11 128.8(11) . . ? C10 N2 H2 115.6 . . ? C11 N2 H2 115.6 . . ? C49 N3 C41 121.6(11) . . ? C49 N3 H3 119.2 . . ? C41 N3 H3 119.2 . . ? C49 N4 C50 128.3(11) . . ? C49 N4 H4 115.9 . . ? C50 N4 H4 115.9 . . ? H3C O3 H3D 104.5 . . ? H4A O4 H4B 104.5 . . ? C2 C1 P1 117.3(8) . . ? C2 C1 H1A 108.0 . . ? P1 C1 H1A 108.0 . . ? C2 C1 H1B 108.0 . . ? P1 C1 H1B 108.0 . . ? H1A C1 H1B 107.2 . . ? N1 C2 C3 111.3(11) . . ? N1 C2 C1 111.0(10) . . ? C3 C2 C1 110.5(10) . . ? N1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C4 C3 C2 111.5(13) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C9 114(2) . . ? C5 C4 C3 127(2) . . ? C9 C4 C3 119.4(15) . . ? C4 C5 C6 126(3) . . ? C4 C5 H5 117.2 . . ? C6 C5 H5 117.2 . . ? C7 C6 C5 117(3) . . ? C7 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? C6 C7 C8 125(3) . . ? C6 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C9 C8 C7 113(3) . . ? C9 C8 H8 123.4 . . ? C7 C8 H8 123.5 . . ? C4 C9 C8 125(2) . . ? C4 C9 H9 117.7 . . ? C8 C9 H9 117.7 . . ? O1 C10 N1 122.3(12) . . ? O1 C10 N2 124.1(11) . . ? N1 C10 N2 113.6(11) . . ? C16 C11 N2 117.6(13) . . ? C16 C11 C12 120.3(13) . . ? N2 C11 C12 121.9(12) . . ? C13 C12 C11 118.1(14) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.9 . . ? C14 C13 C12 121.6(15) . . ? C14 C13 C17 121.1(15) . . ? C12 C13 C17 117.2(15) . . ? C13 C14 C15 119.8(15) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.7(15) . . ? C16 C15 C18' 126(2) . . ? C14 C15 C18' 112(2) . . ? C16 C15 C18 118.0(18) . . ? C14 C15 C18 122.3(19) . . ? C11 C16 C15 120.4(15) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? F1 C17 F3 113(2) . . ? F1 C17 F2 99.7(16) . . ? F3 C17 F2 102(2) . . ? F1 C17 C13 117.0(16) . . ? F3 C17 C13 114.4(16) . . ? F2 C17 C13 108.9(19) . . ? C20 C19 C24 118.5(14) . . ? C20 C19 P1 120.0(11) . . ? C24 C19 P1 120.5(12) . . ? C21 C20 C19 123.2(17) . . ? C21 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? C20 C21 C22 118(2) . . ? C20 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? C23 C22 C21 120.8(17) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 122(2) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C19 C24 C23 117.5(19) . . ? C19 C24 H24 121.2 . . ? C23 C24 H24 121.3 . . ? C26 C25 C30 118.6(15) . . ? C26 C25 P1 122.4(14) . . ? C30 C25 P1 119.0(13) . . ? C25 C26 C27 119(2) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 119(3) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.5 . . ? C29 C28 C27 123(2) . . ? C29 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C28 C29 C30 119(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.5 . . ? C29 C30 C25 121(2) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C32 C31 P1 112.8(9) . . ? C32 C31 H31A 109.0 . . ? P1 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? P1 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C37 C32 C33 120.0(14) . . ? C37 C32 C31 119.8(13) . . ? C33 C32 C31 120.2(14) . . ? C32 C33 C34 118.0(15) . . ? C32 C33 H33 121.0 . . ? C34 C33 H33 121.0 . . ? C36 C37 C32 120.3(14) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C35 C36 C37 121.2(15) . . ? C35 C36 C38 118.7(16) . . ? C37 C36 C38 120.1(15) . . ? C41 C40 P2 117.0(9) . . ? C41 C40 H40A 108.1 . . ? P2 C40 H40A 108.1 . . ? C41 C40 H40B 108.1 . . ? P2 C40 H40B 108.1 . . ? H40A C40 H40B 107.3 . . ? N3 C41 C42 111.9(10) . . ? N3 C41 C40 110.7(10) . . ? C42 C41 C40 110.0(10) . . ? N3 C41 H41 108.0 . . ? C42 C41 H41 108.0 . . ? C40 C41 H41 108.0 . . ? C43 C42 C41 114.8(12) . . ? C43 C42 H42A 108.6 . . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.5 . . ? C44 C43 C48 120.0 . . ? C44 C43 C42 120.9(12) . . ? C48 C43 C42 118.9(12) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? O2 C49 N3 123.9(12) . . ? O2 C49 N4 123.1(12) . . ? N3 C49 N4 113.0(11) . . ? C55 C50 N4 125.1(13) . . ? C55 C50 C51 117.7(13) . . ? N4 C50 C51 117.2(13) . . ? C52 C51 C50 120.7(16) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 122.5(16) . . ? C51 C52 C56 123(2) . . ? C53 C52 C56 114.6(17) . . ? C52 C53 C54 117.6(15) . . ? C52 C53 H53 121.2 . . ? C54 C53 H53 121.2 . . ? C55 C54 C53 120.3(16) . . ? C55 C54 C57 118.3(16) . . ? C53 C54 C57 121.4(17) . . ? C54 C55 C50 121.1(14) . . ? C54 C55 H55 119.5 . . ? C50 C55 H55 119.5 . . ? F15 C56 F14 117(2) . . ? F15 C56 F13 96(2) . . ? F14 C56 F13 93(2) . . ? F15 C56 C52 120(2) . . ? F14 C56 C52 113.2(19) . . ? F13 C56 C52 111(2) . . ? F18 C57 F16 101(3) . . ? F18 C57 F17 97(2) . . ? F16 C57 F17 113.7(19) . . ? F18 C57 C54 116.9(18) . . ? F16 C57 C54 114.3(19) . . ? F17 C57 C54 113(2) . . ? C63 C58 C59 120.1(15) . . ? C63 C58 P2 121.7(12) . . ? C59 C58 P2 117.8(12) . . ? C60 C59 C58 117.6(19) . . ? C60 C59 H59 121.2 . . ? C58 C59 H59 121.2 . . ? C61 C60 C59 127(3) . . ? C61 C60 H60 116.7 . . ? C59 C60 H60 116.7 . . ? C60 C61 C62 119.4(19) . . ? C60 C61 H61 120.3 . . ? C62 C61 H61 120.3 . . ? C61 C62 C63 119(2) . . ? C61 C62 H62 120.7 . . ? C63 C62 H62 120.7 . . ? C58 C63 C62 117(2) . . ? C58 C63 H63 121.3 . . ? C62 C63 H63 121.3 . . ? C69 C64 C65 119.7(14) . . ? C69 C64 P2 118.0(10) . . ? C65 C64 P2 120.4(12) . . ? C64 C65 C66 119.6(19) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 120.0(18) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C68 121(2) . . ? C66 C67 H67 119.3 . . ? C68 C67 H67 119.3 . . ? C67 C68 C69 121(2) . . ? C67 C68 H68 119.5 . . ? C69 C68 H68 119.5 . . ? C64 C69 C68 117.5(17) . . ? C64 C69 H69 121.2 . . ? C68 C69 H69 121.3 . . ? C71 C70 P2 112.6(8) . . ? C71 C70 H70A 109.1 . . ? P2 C70 H70A 109.1 . . ? C71 C70 H70B 109.1 . . ? P2 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? C76 C71 C72 119.1(13) . . ? C76 C71 C70 120.0(12) . . ? C72 C71 C70 120.8(11) . . ? C73 C72 C71 121.0(13) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 121.8(15) . . ? C72 C73 C77 120.6(16) . . ? C74 C73 C77 117.5(16) . . ? C75 C74 C73 116.4(16) . . ? C75 C74 H74 121.8 . . ? C73 C74 H74 121.8 . . ? C74 C75 C76 123.1(14) . . ? C74 C75 C78 119.1(16) . . ? C76 C75 C78 117.7(16) . . ? C71 C76 C75 118.6(14) . . ? C71 C76 H76 120.7 . . ? C75 C76 H76 120.7 . . ? F21 C77 F19 110(2) . . ? F21 C77 F20 93(2) . . ? F19 C77 F20 92(2) . . ? F21 C77 C73 120(2) . . ? F19 C77 C73 119.2(17) . . ? F20 C77 C73 115(2) . . ? F24 C78 F22 110(2) . . ? F24 C78 F23 100(2) . . ? F22 C78 F23 96(2) . . ? F24 C78 C75 120.4(16) . . ? F22 C78 C75 114.0(15) . . ? F23 C78 C75 112.3(18) . . ? F6 C18 F4 104(4) . . ? F6 C18 F5 107(4) . . ? F4 C18 F5 101(3) . . ? F6 C18 C15 113(2) . . ? F4 C18 C15 117(2) . . ? F5 C18 C15 114(2) . . ? F5' C18' F4' 112(4) . . ? F5' C18' F6' 103(5) . . ? F4' C18' F6' 112(4) . . ? F5' C18' C15 104(3) . . ? F4' C18' C15 120(4) . . ? F6' C18' C15 105(3) . . ? C35 C34 C33 121.0(14) . . ? C35 C34 C39 117.0(17) . . ? C33 C34 C39 122.0(19) . . ? C34 C35 C36 119.4(15) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? F7 C38 F9 114(2) . . ? F7 C38 F8 90(2) . . ? F9 C38 F8 90(2) . . ? F7 C38 C36 121.5(18) . . ? F9 C38 C36 119.7(15) . . ? F8 C38 C36 112(2) . . ? C39 F10 F12 51.8(16) . . ? C39 F12 F10 52.0(18) . . ? C39 F11' F12' 72(4) . . ? F11' F12' C39 54(3) . . ? F11 C39 F10 126(3) . . ? F11 C39 F12 110(4) . . ? F10 C39 F12 76(3) . . ? F10' C39 F11' 112(4) . . ? F10' C39 C34 125(4) . . ? F11 C39 C34 112.9(18) . . ? F10 C39 C34 113.5(19) . . ? F12 C39 C34 112(2) . . ? F11' C39 C34 108(3) . . ? F10' C39 F12' 132(5) . . ? F11' C39 F12' 54(3) . . ? C34 C39 F12' 102(2) . . ? 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 P1 C25 1.764(14) . ? P1 C19 1.786(14) . ? P1 C1 1.799(12) . ? P1 C31 1.799(13) . ? P2 C58 1.770(14) . ? P2 C40 1.792(11) . ? P2 C70 1.802(13) . ? P2 C64 1.808(13) . ? N1 C10 1.335(16) . ? N1 C2 1.471(17) . ? N1 H1 0.8600 . ? N2 C10 1.361(17) . ? N2 C11 1.397(18) . ? N2 H2 0.8600 . ? N3 C49 1.334(18) . ? N3 C41 1.472(16) . ? N3 H3 0.8600 . ? N4 C49 1.369(17) . ? N4 C50 1.387(18) . ? N4 H4 0.8600 . ? O1 C10 1.235(15) . ? O2 C49 1.229(16) . ? O3 H3C 0.8499 . ? O3 H3D 0.8500 . ? O4 H4A 0.8500 . ? O4 H4B 0.8500 . ? C1 C2 1.524(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.521(19) . ? C2 H2A 0.9800 . ? C3 C4 1.50(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.35(3) . ? C4 C9 1.38(3) . ? C5 C6 1.40(4) . ? C5 H5 0.9300 . ? C6 C7 1.25(4) . ? C6 H6 0.9300 . ? C7 C8 1.44(4) . ? C7 H7 0.9300 . ? C8 C9 1.40(3) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C16 1.37(2) . ? C11 C12 1.41(2) . ? C12 C13 1.41(2) . ? C12 H12 0.9300 . ? C13 C14 1.36(2) . ? C13 C17 1.49(2) . ? C14 C15 1.39(3) . ? C14 H14 0.9300 . ? C15 C16 1.40(3) . ? C15 C18' 1.46(3) . ? C15 C18 1.47(2) . ? C16 H16 0.9300 . ? C17 F1 1.29(2) . ? C17 F3 1.30(2) . ? C17 F2 1.40(3) . ? C19 C20 1.38(2) . ? C19 C24 1.40(2) . ? C20 C21 1.35(2) . ? C20 H20 0.9300 . ? C21 C22 1.38(3) . ? C21 H21 0.9300 . ? C22 C23 1.34(4) . ? C22 H22 0.9300 . ? C23 C24 1.39(3) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.39(2) . ? C25 C30 1.41(3) . ? C26 C27 1.42(3) . ? C26 H26 0.9300 . ? C27 C28 1.36(5) . ? C27 H27 0.9300 . ? C28 C29 1.33(5) . ? C28 H28 0.9300 . ? C29 C30 1.39(3) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.52(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C37 1.38(2) . ? C32 C33 1.39(2) . ? C33 C34 1.43(2) . ? C33 H33 0.9300 . ? C37 C36 1.37(2) . ? C37 H37 0.9300 . ? C36 C35 1.37(2) . ? C36 C38 1.42(2) . ? C40 C41 1.544(16) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 C42 1.528(19) . ? C41 H41 0.9800 . ? C42 C43 1.453(18) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C50 C55 1.39(2) . ? C50 C51 1.41(2) . ? C51 C52 1.33(2) . ? C51 H51 0.9300 . ? C52 C53 1.39(3) . ? C52 C56 1.46(3) . ? C53 C54 1.40(3) . ? C53 H53 0.9300 . ? C54 C55 1.38(2) . ? C54 C57 1.47(3) . ? C55 H55 0.9300 . ? C56 F15 1.22(3) . ? C56 F14 1.32(3) . ? C56 F13 1.37(3) . ? C57 F18 1.26(3) . ? C57 F16 1.33(3) . ? C57 F17 1.33(3) . ? C58 C63 1.36(2) . ? C58 C59 1.40(2) . ? C59 C60 1.37(3) . ? C59 H59 0.9300 . ? C60 C61 1.21(4) . ? C60 H60 0.9300 . ? C61 C62 1.41(4) . ? C61 H61 0.9300 . ? C62 C63 1.45(3) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 C69 1.36(2) . ? C64 C65 1.36(2) . ? C65 C66 1.42(3) . ? C65 H65 0.9300 . ? C66 C67 1.28(3) . ? C66 H66 0.9300 . ? C67 C68 1.33(4) . ? C67 H67 0.9300 . ? C68 C69 1.42(2) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 C71 1.521(18) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 C76 1.37(2) . ? C71 C72 1.39(2) . ? C72 C73 1.37(2) . ? C72 H72 0.9300 . ? C73 C74 1.39(2) . ? C73 C77 1.40(2) . ? C74 C75 1.37(3) . ? C74 H74 0.9300 . ? C75 C76 1.42(2) . ? C75 C78 1.45(2) . ? C76 H76 0.9300 . ? C77 F21 1.24(2) . ? C77 F19 1.30(2) . ? C77 F20 1.34(2) . ? C78 F24 1.25(2) . ? C78 F22 1.33(2) . ? C78 F23 1.35(2) . ? C18 F6 1.32(3) . ? C18 F4 1.33(3) . ? C18 F5 1.34(3) . ? C18' F5' 1.33(3) . ? C18' F4' 1.33(3) . ? C18' F6' 1.34(3) . ? F7 C38 1.23(2) . ? F9 C38 1.29(2) . ? C34 C35 1.36(3) . ? C34 C39 1.48(2) . ? C35 H35 0.9300 . ? F8 C38 1.33(2) . ? F10 C39 1.32(2) . ? F10 F12 1.63(6) . ? F11 C39 1.29(2) . ? F12 C39 1.32(3) . ? F10' C39 1.13(5) . ? F11' C39 1.36(6) . ? F11' F12' 1.35(7) . ? F12' C39 1.59(6) . ? 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 C25 P1 C1 C2 -65.7(11) . . . . ? C19 P1 C1 C2 59.1(11) . . . . ? C31 P1 C1 C2 173.7(10) . . . . ? C10 N1 C2 C3 108.1(14) . . . . ? C10 N1 C2 C1 -128.4(12) . . . . ? P1 C1 C2 N1 71.4(12) . . . . ? P1 C1 C2 C3 -164.7(10) . . . . ? N1 C2 C3 C4 -176.0(12) . . . . ? C1 C2 C3 C4 60.2(16) . . . . ? C2 C3 C4 C5 -110(2) . . . . ? C2 C3 C4 C9 66.8(18) . . . . ? C9 C4 C5 C6 6(4) . . . . ? C3 C4 C5 C6 -177(2) . . . . ? C4 C5 C6 C7 -15(5) . . . . ? C5 C6 C7 C8 15(5) . . . . ? C6 C7 C8 C9 -7(4) . . . . ? C5 C4 C9 C8 3(3) . . . . ? C3 C4 C9 C8 -174.2(18) . . . . ? C7 C8 C9 C4 -3(3) . . . . ? C2 N1 C10 O1 0(2) . . . . ? C2 N1 C10 N2 177.3(12) . . . . ? C11 N2 C10 O1 4(2) . . . . ? C11 N2 C10 N1 -172.7(14) . . . . ? C10 N2 C11 C16 172.0(16) . . . . ? C10 N2 C11 C12 -4(3) . . . . ? C16 C11 C12 C13 3(2) . . . . ? N2 C11 C12 C13 178.7(15) . . . . ? C11 C12 C13 C14 -1(3) . . . . ? C11 C12 C13 C17 175.4(18) . . . . ? C12 C13 C14 C15 -2(3) . . . . ? C17 C13 C14 C15 -178(2) . . . . ? C13 C14 C15 C16 3(3) . . . . ? C13 C14 C15 C18' 166(3) . . . . ? C13 C14 C15 C18 -176(2) . . . . ? N2 C11 C16 C15 -177.6(18) . . . . ? C12 C11 C16 C15 -1(3) . . . . ? C14 C15 C16 C11 -1(3) . . . . ? C18' C15 C16 C11 -162(3) . . . . ? C18 C15 C16 C11 177(2) . . . . ? C14 C13 C17 F1 141.4(19) . . . . ? C12 C13 C17 F1 -35(3) . . . . ? C14 C13 C17 F3 7(3) . . . . ? C12 C13 C17 F3 -170(2) . . . . ? C14 C13 C17 F2 -107(2) . . . . ? C12 C13 C17 F2 77(2) . . . . ? C25 P1 C19 C20 146.5(12) . . . . ? C1 P1 C19 C20 21.7(14) . . . . ? C31 P1 C19 C20 -93.9(13) . . . . ? C25 P1 C19 C24 -45.3(15) . . . . ? C1 P1 C19 C24 -170.1(12) . . . . ? C31 P1 C19 C24 74.3(14) . . . . ? C24 C19 C20 C21 0(2) . . . . ? P1 C19 C20 C21 168.6(13) . . . . ? C19 C20 C21 C22 2(3) . . . . ? C20 C21 C22 C23 -2(3) . . . . ? C21 C22 C23 C24 0(3) . . . . ? C20 C19 C24 C23 -2(2) . . . . ? P1 C19 C24 C23 -170.0(13) . . . . ? C22 C23 C24 C19 1(3) . . . . ? C19 P1 C25 C26 -24.8(15) . . . . ? C1 P1 C25 C26 99.6(13) . . . . ? C31 P1 C25 C26 -141.6(13) . . . . ? C19 P1 C25 C30 158.4(14) . . . . ? C1 P1 C25 C30 -77.3(15) . . . . ? C31 P1 C25 C30 41.6(15) . . . . ? C30 C25 C26 C27 -1(2) . . . . ? P1 C25 C26 C27 -177.9(14) . . . . ? C25 C26 C27 C28 4(3) . . . . ? C26 C27 C28 C29 -5(5) . . . . ? C27 C28 C29 C30 3(5) . . . . ? C28 C29 C30 C25 1(4) . . . . ? C26 C25 C30 C29 -2(3) . . . . ? P1 C25 C30 C29 175.3(18) . . . . ? C25 P1 C31 C32 177.8(10) . . . . ? C19 P1 C31 C32 57.2(11) . . . . ? C1 P1 C31 C32 -60.8(11) . . . . ? P1 C31 C32 C37 -82.4(14) . . . . ? P1 C31 C32 C33 98.2(13) . . . . ? C37 C32 C33 C34 -0.2(19) . . . . ? C31 C32 C33 C34 179.2(12) . . . . ? C33 C32 C37 C36 -2(2) . . . . ? C31 C32 C37 C36 178.2(13) . . . . ? C32 C37 C36 C35 4(2) . . . . ? C32 C37 C36 C38 -176.2(17) . . . . ? C58 P2 C40 C41 -63.4(11) . . . . ? C70 P2 C40 C41 176.9(9) . . . . ? C64 P2 C40 C41 61.0(11) . . . . ? C49 N3 C41 C42 102.6(14) . . . . ? C49 N3 C41 C40 -134.3(12) . . . . ? P2 C40 C41 N3 67.1(12) . . . . ? P2 C40 C41 C42 -168.7(10) . . . . ? N3 C41 C42 C43 -175.9(12) . . . . ? C40 C41 C42 C43 60.6(17) . . . . ? C41 C42 C43 C44 55.7(16) . . . . ? C41 C42 C43 C48 -120.2(14) . . . . ? C48 C43 C44 C45 0.0 . . . . ? C42 C43 C44 C45 -175.8(11) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 C47 0.0 . . . . ? C42 C43 C48 C47 175.9(11) . . . . ? C41 N3 C49 O2 6.1(18) . . . . ? C41 N3 C49 N4 -176.8(10) . . . . ? C50 N4 C49 O2 3(2) . . . . ? C50 N4 C49 N3 -174.2(13) . . . . ? C49 N4 C50 C55 7(2) . . . . ? C49 N4 C50 C51 -171.4(13) . . . . ? C55 C50 C51 C52 1(2) . . . . ? N4 C50 C51 C52 -179.9(14) . . . . ? C50 C51 C52 C53 1(3) . . . . ? C50 C51 C52 C56 -177.6(18) . . . . ? C51 C52 C53 C54 -3(3) . . . . ? C56 C52 C53 C54 175.3(19) . . . . ? C52 C53 C54 C55 4(3) . . . . ? C52 C53 C54 C57 -176(2) . . . . ? C53 C54 C55 C50 -2(3) . . . . ? C57 C54 C55 C50 178.4(19) . . . . ? N4 C50 C55 C54 -179.5(15) . . . . ? C51 C50 C55 C54 -1(2) . . . . ? C51 C52 C56 F15 -140(3) . . . . ? C53 C52 C56 F15 41(3) . . . . ? C51 C52 C56 F14 74(3) . . . . ? C53 C52 C56 F14 -104(3) . . . . ? C51 C52 C56 F13 -29(3) . . . . ? C53 C52 C56 F13 152(2) . . . . ? C55 C54 C57 F18 -42(3) . . . . ? C53 C54 C57 F18 138(2) . . . . ? C55 C54 C57 F16 -159(2) . . . . ? C53 C54 C57 F16 21(3) . . . . ? C55 C54 C57 F17 69(3) . . . . ? C53 C54 C57 F17 -111(2) . . . . ? C40 P2 C58 C63 100.0(13) . . . . ? C70 P2 C58 C63 -142.5(12) . . . . ? C64 P2 C58 C63 -24.2(14) . . . . ? C40 P2 C58 C59 -72.5(14) . . . . ? C70 P2 C58 C59 45.0(14) . . . . ? C64 P2 C58 C59 163.4(13) . . . . ? C63 C58 C59 C60 2(3) . . . . ? P2 C58 C59 C60 175.1(15) . . . . ? C58 C59 C60 C61 -5(4) . . . . ? C59 C60 C61 C62 6(4) . . . . ? C60 C61 C62 C63 -5(3) . . . . ? C59 C58 C63 C62 -2(2) . . . . ? P2 C58 C63 C62 -174.2(12) . . . . ? C61 C62 C63 C58 3(3) . . . . ? C58 P2 C64 C69 147.5(11) . . . . ? C40 P2 C64 C69 23.2(12) . . . . ? C70 P2 C64 C69 -92.4(11) . . . . ? C58 P2 C64 C65 -48.0(13) . . . . ? C40 P2 C64 C65 -172.3(11) . . . . ? C70 P2 C64 C65 72.1(13) . . . . ? C69 C64 C65 C66 -6(2) . . . . ? P2 C64 C65 C66 -170.3(13) . . . . ? C64 C65 C66 C67 10(3) . . . . ? C65 C66 C67 C68 -10(4) . . . . ? C66 C67 C68 C69 7(4) . . . . ? C65 C64 C69 C68 3(2) . . . . ? P2 C64 C69 C68 167.9(13) . . . . ? C67 C68 C69 C64 -4(3) . . . . ? C58 P2 C70 C71 177.1(9) . . . . ? C40 P2 C70 C71 -62.5(10) . . . . ? C64 P2 C70 C71 56.1(10) . . . . ? P2 C70 C71 C76 93.7(13) . . . . ? P2 C70 C71 C72 -82.9(13) . . . . ? C76 C71 C72 C73 0(2) . . . . ? C70 C71 C72 C73 176.3(13) . . . . ? C71 C72 C73 C74 2(2) . . . . ? C71 C72 C73 C77 177.9(16) . . . . ? C72 C73 C74 C75 -2(2) . . . . ? C77 C73 C74 C75 -178.3(16) . . . . ? C73 C74 C75 C76 1(2) . . . . ? C73 C74 C75 C78 177.6(16) . . . . ? C72 C71 C76 C75 -0.8(19) . . . . ? C70 C71 C76 C75 -177.4(11) . . . . ? C74 C75 C76 C71 0(2) . . . . ? C78 C75 C76 C71 -176.3(15) . . . . ? C72 C73 C77 F21 174(2) . . . . ? C74 C73 C77 F21 -10(3) . . . . ? C72 C73 C77 F19 32(3) . . . . ? C74 C73 C77 F19 -152(2) . . . . ? C72 C73 C77 F20 -77(3) . . . . ? C74 C73 C77 F20 100(2) . . . . ? C74 C75 C78 F24 157(2) . . . . ? C76 C75 C78 F24 -26(3) . . . . ? C74 C75 C78 F22 -69(3) . . . . ? C76 C75 C78 F22 108(2) . . . . ? C74 C75 C78 F23 39(2) . . . . ? C76 C75 C78 F23 -143.8(19) . . . . ? C16 C15 C18 F6 -74(4) . . . . ? C14 C15 C18 F6 104(4) . . . . ? C18' C15 C18 F6 166(8) . . . . ? C16 C15 C18 F4 165(4) . . . . ? C14 C15 C18 F4 -16(5) . . . . ? C18' C15 C18 F4 45(7) . . . . ? C16 C15 C18 F5 48(4) . . . . ? C14 C15 C18 F5 -134(3) . . . . ? C18' C15 C18 F5 -72(8) . . . . ? C16 C15 C18' F5' -39(6) . . . . ? C14 C15 C18' F5' 159(4) . . . . ? C18 C15 C18' F5' 32(6) . . . . ? C16 C15 C18' F4' 87(5) . . . . ? C14 C15 C18' F4' -75(5) . . . . ? C18 C15 C18' F4' 158(10) . . . . ? C16 C15 C18' F6' -147(4) . . . . ? C14 C15 C18' F6' 51(4) . . . . ? C18 C15 C18' F6' -76(8) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C32 C33 C34 C39 -177.1(15) . . . . ? C33 C34 C35 C36 -1(2) . . . . ? C39 C34 C35 C36 178.2(15) . . . . ? C37 C36 C35 C34 -2(2) . . . . ? C38 C36 C35 C34 177.7(17) . . . . ? C35 C36 C38 F7 -10(4) . . . . ? C37 C36 C38 F7 170(3) . . . . ? C35 C36 C38 F9 -163(2) . . . . ? C37 C36 C38 F9 17(3) . . . . ? C35 C36 C38 F8 94(2) . . . . ? C37 C36 C38 F8 -86(2) . . . . ? F12 F10 C39 F10' -134(4) . . . . ? F12 F10 C39 F11 -104(4) . . . . ? F12 F10 C39 F11' -44(5) . . . . ? F12 F10 C39 C34 108(3) . . . . ? F12 F10 C39 F12' 2(3) . . . . ? F10 F12 C39 F10' 42(5) . . . . ? F10 F12 C39 F11 124(4) . . . . ? F10 F12 C39 F11' 148(3) . . . . ? F10 F12 C39 C34 -110(2) . . . . ? F10 F12 C39 F12' -175(9) . . . . ? F12' F11' C39 F10' 127(7) . . . . ? F12' F11' C39 F11 164(4) . . . . ? F12' F11' C39 F10 62(5) . . . . ? F12' F11' C39 F12 16(3) . . . . ? F12' F11' C39 C34 -91(3) . . . . ? C35 C34 C39 F10' -15(8) . . . . ? C33 C34 C39 F10' 164(8) . . . . ? C35 C34 C39 F11 -101(4) . . . . ? C33 C34 C39 F11 77(4) . . . . ? C35 C34 C39 F10 50(3) . . . . ? C33 C34 C39 F10 -131(2) . . . . ? C35 C34 C39 F12 134(3) . . . . ? C33 C34 C39 F12 -47(3) . . . . ? C35 C34 C39 F11' -151(4) . . . . ? C33 C34 C39 F11' 28(4) . . . . ? C35 C34 C39 F12' 154(2) . . . . ? C33 C34 C39 F12' -27(3) . . . . ? F11' F12' C39 F10' -88(8) . . . . ? F11' F12' C39 F11 -12(3) . . . . ? F11' F12' C39 F10 -140(3) . . . . ? F11' F12' C39 F12 -135(10) . . . . ? F11' F12' C39 C34 104(3) . . . . ?