#------------------------------------------------------------------------------ #$Date: 2021-07-05 21:13:41 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267243 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158105.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_7158105 loop_ _publ_author_name 'Li, Jun' 'Daniliuc, Constantin G.' 'Kehr, Gerald' 'Erker, Gerhard' _publ_section_title ; Formation of amidino-borate derivatives by a multi-component reaction. ; _journal_issue 25 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 5551 _journal_page_last 5554 _journal_paper_doi 10.1039/d1ob00775k _journal_volume 19 _journal_year 2021 _chemical_formula_sum 'C41 H39 B F9 N3' _chemical_formula_weight 755.56 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_method 'APEX3 v2016.1-0' _audit_update_record ; 2021-02-23 deposited with the CCDC. 2021-06-01 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.6283(7) _cell_length_b 8.9160(2) _cell_length_c 19.7224(4) _cell_measurement_reflns_used 6705 _cell_measurement_temperature 173.(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 4.08 _cell_volume 3627.38(16) _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_collection ; Collect (Nonius B.V., 1998) ; _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'XP (Sheldrick, 2014)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 173.(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'rotating anode Nonius FR591' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'Montel mirror' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 21027 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 4.08 _diffrn_source 'Mo rotating anode' _diffrn_source_type 'Mo rotating anode' _exptl_absorpt_coefficient_mu 0.113 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.99 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1568 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.352 _refine_diff_density_min -0.250 _refine_ls_abs_structure_details ; Flack x determined using 1824 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.0(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 600 _refine_ls_number_reflns 6341 _refine_ls_number_restraints 302 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0781 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+6.3280P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1810 _refine_ls_wR_factor_ref 0.2025 _reflns_number_gt 5202 _reflns_number_total 6341 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob00775k2.cif _cod_data_source_block erk9465 _cod_depositor_comments 'Adding full bibliography for 7158104--7158107.cif.' _cod_database_code 7158105 _shelx_res_file ; erk9465.res created by SHELXL-2014/7 TITL erk9465 in P2(1)2(1)2(1) CELL 0.71073 20.6283 8.9160 19.7224 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0002 0.0004 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H B N F UNIT 164 156 4 12 36 SIZE 0.10 0.09 0.04 TEMP -100 ACTA CONF OMIT -3 50 OMIT 0 3 3 OMIT 0 6 0 L.S. 20 BOND $H FMAP 2 PLAN 10 WGHT 0.078400 6.328000 FVAR 0.19949 0.77466 0.67386 N1 4 0.833621 0.709859 0.628463 11.00000 0.02902 0.04582 = 0.02727 0.00070 0.00498 -0.00237 N3 4 0.995596 0.699097 0.565162 11.00000 0.02656 0.04733 = 0.03202 0.00421 0.00089 0.00128 C1 1 0.933324 0.720877 0.698429 11.00000 0.03584 0.04522 = 0.02993 -0.00062 0.00122 -0.00105 C2 1 0.904635 0.720452 0.769801 11.00000 0.04697 0.07466 = 0.02221 -0.00281 0.00071 0.00331 AFIX 23 H2A 2 0.884979 0.818828 0.780720 11.00000 -1.20000 H2B 2 0.871190 0.641481 0.774440 11.00000 -1.20000 AFIX 0 C3 1 0.962277 0.688529 0.815594 11.00000 0.05834 0.06351 = 0.03138 0.00509 -0.01193 0.00201 AFIX 23 H3A 2 0.955436 0.731563 0.861311 11.00000 -1.20000 H3B 2 0.969719 0.579258 0.819943 11.00000 -1.20000 AFIX 0 C4 1 1.017906 0.762752 0.780759 11.00000 0.04266 0.06635 = 0.03549 -0.00184 -0.01126 0.00102 AFIX 23 H4A 2 1.059648 0.718847 0.795578 11.00000 -1.20000 H4B 2 1.018378 0.871842 0.790103 11.00000 -1.20000 AFIX 0 C5 1 1.005847 0.732180 0.705609 11.00000 0.03283 0.04450 = 0.04188 0.00073 -0.00701 -0.00096 AFIX 23 H5A 2 1.023037 0.815038 0.677443 11.00000 -1.20000 H5B 2 1.026934 0.637427 0.691525 11.00000 -1.20000 AFIX 0 C7 1 0.903001 0.712078 0.637788 11.00000 0.02859 0.04488 = 0.02910 0.00323 0.00007 -0.00273 C8 1 0.933490 0.701563 0.568709 11.00000 0.03665 0.03453 = 0.02705 0.00374 0.00070 -0.00175 C9 1 0.814917 0.698143 0.563492 11.00000 0.03333 0.03133 = 0.03161 0.00126 -0.00010 0.00057 C11 1 0.788965 0.747733 0.682789 11.00000 0.02792 0.04929 = 0.02519 -0.00545 0.00230 -0.00137 C12 1 0.780896 0.899016 0.699439 11.00000 0.04810 0.04748 = 0.03312 -0.00658 -0.00075 -0.00461 C13 1 0.739760 0.932614 0.752731 11.00000 0.04473 0.06094 = 0.05230 -0.01950 -0.00173 0.00033 AFIX 43 H13 2 0.733447 1.034365 0.765408 11.00000 -1.20000 AFIX 0 C14 1 0.708268 0.822924 0.787223 11.00000 0.04519 0.09474 = 0.04311 -0.01837 0.00806 -0.00228 AFIX 43 H14 2 0.680302 0.849290 0.823590 11.00000 -1.20000 AFIX 0 C15 1 0.716059 0.674980 0.770575 11.00000 0.04723 0.08009 = 0.04121 0.00573 0.01354 -0.01392 AFIX 43 H15 2 0.693979 0.600338 0.796036 11.00000 -1.20000 AFIX 0 C16 1 0.756683 0.631215 0.715766 11.00000 0.04970 0.05365 = 0.03284 -0.00595 0.00318 -0.01026 C17 1 0.819360 1.019313 0.664883 11.00000 0.06334 0.04147 = 0.06039 -0.00837 0.00363 -0.00714 AFIX 137 H17A 2 0.826305 0.991766 0.617331 11.00000 -1.50000 H17B 2 0.861348 1.030517 0.687573 11.00000 -1.50000 H17C 2 0.795589 1.114348 0.667141 11.00000 -1.50000 AFIX 0 C18 1 0.765665 0.470600 0.698301 11.00000 0.06962 0.04944 = 0.05673 0.01217 0.01219 -0.00806 AFIX 137 H18A 2 0.739356 0.445943 0.658456 11.00000 -1.50000 H18B 2 0.752101 0.408154 0.736653 11.00000 -1.50000 H18C 2 0.811469 0.451671 0.688265 11.00000 -1.50000 AFIX 0 SIMU 0.02 0.04 0.9 N2 > C28A SAME N2 C21A > C28A SADI N2 C21 SADI c21 c22 c22 c23 c23 c24 c24 c25 c25 c26 SADI c22 c27 c26 c28 ISOR 0.007 C21 > C28A N2 4 0.750987 0.703505 0.550674 11.00000 0.02538 0.04586 = 0.02913 -0.00134 0.00071 0.00217 H2 2 0.720757 0.743781 0.583957 11.00000 0.04278 PART 1 31 C21 1 0.721306 0.730484 0.484179 31.00000 0.02351 0.04590 = 0.03032 -0.00672 0.00592 0.00475 C22 1 0.717889 0.875877 0.459262 31.00000 0.03159 0.03712 = 0.04110 -0.00514 0.00544 0.00168 C23 1 0.688049 0.899319 0.396947 31.00000 0.03337 0.04163 = 0.04715 0.00975 0.00701 0.00431 AFIX 43 H23 2 0.683997 0.998436 0.379787 31.00000 -1.20000 AFIX 0 C24 1 0.664199 0.780190 0.359638 31.00000 0.03694 0.04723 = 0.03740 -0.00261 0.00244 -0.00097 AFIX 43 H24 2 0.645520 0.797637 0.316322 31.00000 -1.20000 AFIX 0 C25 1 0.667369 0.636148 0.384949 31.00000 0.04831 0.04265 = 0.04248 -0.00042 -0.00285 -0.00222 AFIX 43 H25 2 0.649096 0.555393 0.360006 31.00000 -1.20000 AFIX 0 C26 1 0.697188 0.609097 0.446737 31.00000 0.03949 0.03874 = 0.04182 -0.00163 0.00520 0.00235 C27 1 0.743985 1.005811 0.499056 31.00000 0.05729 0.04106 = 0.06767 -0.00474 -0.00353 -0.00292 AFIX 33 H27A 2 0.737272 1.098765 0.473485 31.00000 -1.50000 H27B 2 0.721296 1.012347 0.542613 31.00000 -1.50000 H27C 2 0.790445 0.991252 0.507083 31.00000 -1.50000 AFIX 0 C28 1 0.696189 0.448828 0.473693 31.00000 0.05584 0.05140 = 0.06975 -0.00564 -0.01007 -0.01320 AFIX 33 H28A 2 0.718722 0.444952 0.517402 31.00000 -1.50000 H28B 2 0.651190 0.416137 0.479649 31.00000 -1.50000 H28C 2 0.718011 0.382389 0.441351 31.00000 -1.50000 AFIX 0 PART 2 -31 C21A 1 0.722959 0.702667 0.482713 -31.00000 0.02459 0.03607 = 0.03382 0.00210 0.00062 0.00576 C22A 1 0.712935 0.839261 0.450670 -31.00000 0.03204 0.03534 = 0.03816 -0.00397 0.00245 0.00214 C23A 1 0.681631 0.842271 0.388347 -31.00000 0.03742 0.03845 = 0.03546 -0.00268 -0.00229 -0.00232 AFIX 43 H23A 2 0.673898 0.934311 0.365466 -31.00000 -1.20000 AFIX 0 C24A 1 0.662238 0.708463 0.360860 -31.00000 0.03360 0.03772 = 0.03660 -0.00408 -0.00046 -0.00063 AFIX 43 H24A 2 0.646325 0.706191 0.315670 -31.00000 -1.20000 AFIX 0 C25A 1 0.665371 0.577691 0.397379 -31.00000 0.04673 0.04847 = 0.04821 -0.00595 0.00098 -0.00242 AFIX 43 H25A 2 0.648227 0.488477 0.378090 -31.00000 -1.20000 AFIX 0 C26A 1 0.692455 0.571594 0.460841 -31.00000 0.03033 0.03487 = 0.03580 0.00098 -0.00139 -0.00330 C27A 1 0.739776 0.981093 0.480840 -31.00000 0.03992 0.05228 = 0.02172 -0.01502 0.01439 0.01083 AFIX 33 H27D 2 0.728280 1.066405 0.451909 -31.00000 -1.50000 H27E 2 0.721482 0.995964 0.526203 -31.00000 -1.50000 H27F 2 0.787065 0.973372 0.484078 -31.00000 -1.50000 AFIX 0 C28A 1 0.690040 0.429831 0.502077 -31.00000 0.06605 0.04643 = 0.09141 -0.01143 -0.00187 0.00560 AFIX 33 H28D 2 0.711660 0.446341 0.545689 -31.00000 -1.50000 H28E 2 0.644751 0.401578 0.509952 -31.00000 -1.50000 H28F 2 0.712137 0.349191 0.477461 -31.00000 -1.50000 AFIX 0 PART 0 C31 1 1.028681 0.698481 0.501897 11.00000 0.02203 0.04524 = 0.03305 0.00221 -0.00195 -0.00120 C32 1 1.059584 0.567577 0.479528 11.00000 0.03081 0.04625 = 0.03900 -0.00668 -0.00002 -0.00076 C33 1 1.093732 0.570975 0.419039 11.00000 0.03413 0.06176 = 0.04634 -0.01331 -0.00398 0.00008 AFIX 43 H33 2 1.112658 0.481343 0.402115 11.00000 -1.20000 AFIX 0 C34 1 1.100668 0.703473 0.382839 11.00000 0.03701 0.07796 = 0.03192 -0.00405 -0.00011 -0.00074 AFIX 43 H34 2 1.123183 0.704316 0.340821 11.00000 -1.20000 AFIX 0 C35 1 1.074579 0.833469 0.408497 11.00000 0.04002 0.05739 = 0.03635 0.01072 -0.00023 -0.00100 AFIX 43 H35 2 1.081077 0.925350 0.385073 11.00000 -1.20000 AFIX 0 C36 1 1.038756 0.832409 0.468341 11.00000 0.03468 0.04478 = 0.04590 -0.00072 -0.00297 -0.00232 C37 1 1.058551 0.425125 0.521206 11.00000 0.04036 0.04336 = 0.06835 -0.00112 -0.00908 0.00594 AFIX 137 H37A 2 1.102045 0.405405 0.539099 11.00000 -1.50000 H37B 2 1.044896 0.341024 0.492578 11.00000 -1.50000 H37C 2 1.028044 0.436679 0.558938 11.00000 -1.50000 AFIX 0 C38 1 1.012763 0.978849 0.497108 11.00000 0.05076 0.04234 = 0.05872 0.00291 0.00640 0.00508 AFIX 137 H38A 2 1.030038 0.993944 0.542891 11.00000 -1.50000 H38B 2 0.965325 0.974649 0.498996 11.00000 -1.50000 H38C 2 1.026182 1.062294 0.467970 11.00000 -1.50000 AFIX 0 B1 3 0.875529 0.698551 0.512328 11.00000 0.02993 0.03581 = 0.02881 0.00206 0.00252 0.00196 H1 2 0.874648 0.817778 0.490612 11.00000 0.03422 C41 1 0.887360 0.571842 0.453589 11.00000 0.01912 0.04281 = 0.02761 0.00107 -0.00001 0.00116 C42 1 0.901739 0.614786 0.385198 11.00000 0.03271 0.03772 = 0.03034 -0.00306 -0.00022 0.00250 C43 1 0.930439 0.519266 0.339604 11.00000 0.03008 0.05526 = 0.03377 0.00507 -0.00030 -0.00563 AFIX 43 H43 2 0.941268 0.554790 0.295626 11.00000 -1.20000 AFIX 0 C45 1 0.924157 0.319166 0.419868 11.00000 0.03716 0.04318 = 0.03272 0.00228 0.00001 -0.00135 AFIX 43 H45 2 0.929040 0.215943 0.430664 11.00000 -1.20000 AFIX 0 C46 1 0.897553 0.417682 0.466754 11.00000 0.02991 0.03624 = 0.03104 -0.00175 -0.00067 -0.00322 C47 1 0.883605 0.766909 0.358174 11.00000 0.03125 0.05322 = 0.03220 0.00473 -0.00068 0.00507 F1 5 0.923484 0.877167 0.376380 11.00000 0.05625 0.04872 = 0.06352 0.01621 -0.00562 -0.00641 F2 5 0.823653 0.810041 0.376136 11.00000 0.03850 0.07293 = 0.04710 0.01983 0.01141 0.01905 F3 5 0.882735 0.766401 0.289866 11.00000 0.06227 0.07144 = 0.03031 0.01552 0.00779 0.01897 C44 1 0.943686 0.373568 0.356575 11.00000 0.03674 0.04929 = 0.03060 -0.00449 0.00600 0.00602 ISOR 0.008 C48 > F6 C48 1 0.979255 0.270775 0.309781 11.00000 0.05062 0.05664 = 0.03629 -0.00097 0.00810 0.00631 F4 5 0.986547 0.327236 0.248665 11.00000 0.09628 0.08041 = 0.03711 -0.00098 0.02109 0.01776 F5 5 0.949859 0.141134 0.300568 11.00000 0.11373 0.06030 = 0.10224 -0.02926 0.05404 -0.00522 F6 5 1.037742 0.237212 0.332354 11.00000 0.06301 0.13789 = 0.05753 -0.01933 -0.00245 0.04596 SIMU 0.02 0.04 0.9 c49 > f9a SAME c49 f7a f8a f9a SADI c49 f7 c49 f8 c49 f9 SADI f7 f8 f7 f9 f8 f9 ISOR 0.008 f7 > f9a C49 1 0.878983 0.345364 0.533498 11.00000 0.03457 0.03735 = 0.03609 -0.00329 0.00822 -0.00486 PART 1 21 F7 5 0.890159 0.200947 0.536207 21.00000 0.09977 0.03694 = 0.04454 0.00790 0.02933 0.00851 F8 5 0.908091 0.406615 0.587298 21.00000 0.08429 0.06211 = 0.02662 0.00982 -0.01444 -0.03367 F9 5 0.816143 0.361459 0.547135 21.00000 0.04177 0.10129 = 0.05157 0.02803 0.01356 0.01345 PART 2 -21 F7A 5 0.927679 0.263440 0.559220 -21.00000 0.06537 0.09588 = 0.06172 0.02625 -0.00015 0.00900 F8A 5 0.855172 0.426055 0.582056 -21.00000 0.12160 0.07760 = 0.07569 0.01240 0.03515 -0.00657 F9A 5 0.832984 0.239757 0.521748 -21.00000 0.07903 0.08177 = 0.08364 -0.01169 -0.00645 -0.01624 PART 0 HKLF 4 1 0 0 1 1 0 0 0 1 0 REM erk9465 in P2(1)2(1)2(1) REM R1 = 0.0781 for 5202 Fo > 4sig(Fo) and 0.1019 for all 6341 data REM 600 parameters refined using 302 restraints END WGHT 0.0784 6.3149 REM Highest difference peak 0.352, deepest hole -0.250, 1-sigma level 0.060 Q1 1 0.8276 0.6877 0.3823 11.00000 0.05 0.35 Q2 1 0.9838 0.1724 0.2470 11.00000 0.05 0.30 Q3 1 0.9590 0.8089 0.8156 11.00000 0.05 0.29 Q4 1 0.8267 0.1433 0.5554 11.00000 0.05 0.27 Q5 1 1.0611 1.0601 0.5149 11.00000 0.05 0.27 Q6 1 1.0001 0.8083 0.5737 11.00000 0.05 0.27 Q7 1 0.8410 0.8287 0.6238 11.00000 0.05 0.26 Q8 1 1.0725 0.9378 0.4780 11.00000 0.05 0.25 Q9 1 0.9375 0.3434 0.2853 11.00000 0.05 0.24 Q10 1 0.8960 0.1011 0.4607 11.00000 0.05 0.24 ; _shelx_res_checksum 57844 _shelx_hkl_file ; 0 0 5 0.10 0.30 1 0 0 6 491.10 8.40 1 0 0 7 1.60 0.30 1 0 0 8 138.10 3.20 1 0 0 9 0.50 0.30 1 0 0 10 173.50 4.40 1 0 0 11 1.00 0.50 1 0 0 12 58.30 1.90 1 0 0 13 1.90 0.50 1 0 0 14 110.80 3.20 1 0 0 15 0.80 0.60 1 0 0 17 0.60 0.60 1 0 0 18 40.60 1.70 1 0 0 19 2.40 0.70 1 0 0 20 7.90 0.80 1 0 0 21 0.00 0.40 1 0 0 22 8.90 0.90 1 0 0 23 0.20 0.60 1 0 0 24 1.20 0.60 1 0 0 25 0.50 0.50 1 0 1 4 23.70 0.40 1 0 1 5 501.30 6.20 1 0 1 6 878.90 16.80 1 0 1 7 67.00 1.00 1 0 1 8 207.40 2.60 1 0 1 9 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0.20 1 -1 -5 -3 7.30 0.20 1 1 5 4 80.90 1.60 1 -1 -5 -4 81.70 1.30 1 1 5 5 165.00 2.40 1 -1 -5 -5 161.10 2.10 1 1 5 6 109.20 1.60 1 -1 -5 -6 103.40 1.90 1 1 5 7 25.30 0.50 1 -1 -5 -7 26.70 0.50 1 1 5 8 155.40 3.30 1 -1 -5 -8 155.80 2.30 1 1 5 9 38.20 0.90 1 -1 -5 -9 35.20 0.70 1 1 5 10 36.60 0.80 1 -1 -5 -10 34.00 0.70 1 1 5 11 80.60 1.60 1 -1 -5 -11 83.60 1.60 1 1 5 12 43.00 0.90 1 -1 -5 -12 44.70 1.10 1 1 5 13 44.80 1.30 1 -1 -5 -13 41.00 1.00 1 1 5 14 53.90 1.20 1 -1 -5 -14 56.80 1.70 1 1 5 15 2.10 0.30 1 -1 -5 -15 2.80 0.40 1 1 5 16 5.30 0.60 1 -1 -5 -16 4.80 0.40 1 1 5 17 28.20 0.90 1 -1 -5 -17 27.70 1.00 1 1 5 18 8.70 0.70 1 -1 -5 -18 9.00 0.60 1 1 5 19 2.80 0.40 1 -1 -5 -19 3.50 0.50 1 1 5 20 7.90 0.80 1 -1 -5 -20 7.00 0.50 1 1 5 21 6.60 0.70 1 -1 -5 -21 3.10 0.50 1 1 5 22 5.70 0.60 1 -1 -5 -22 7.00 0.70 1 1 5 23 3.60 0.60 1 -1 -5 -23 1.90 0.50 1 1 5 24 1.00 0.60 1 -1 -5 -24 1.50 0.70 1 1 5 25 -0.20 0.50 1 -1 -5 -25 0.30 0.50 1 1 6 0 20.90 0.40 1 1 6 1 31.30 0.50 1 -1 -6 -1 29.70 0.50 1 1 6 2 98.00 1.40 1 -1 -6 -2 89.70 1.50 1 1 6 3 45.90 0.70 1 -1 -6 -3 45.20 0.70 1 1 6 4 131.90 1.90 1 -1 -6 -4 130.30 1.90 1 1 6 5 183.60 2.70 1 -1 -6 -5 177.80 2.80 1 1 6 6 24.40 0.50 1 -1 -6 -6 26.00 0.50 1 1 6 7 256.70 3.60 1 -1 -6 -7 238.00 4.30 1 1 6 8 44.20 0.80 1 -1 -6 -8 42.70 0.90 1 1 6 9 52.60 1.00 1 -1 -6 -9 52.10 0.80 1 1 6 10 54.00 0.90 1 -1 -6 -10 56.20 0.90 1 1 6 11 5.80 0.30 1 -1 -6 -11 5.30 0.20 1 1 6 12 0.10 0.20 1 -1 -6 -12 0.20 0.10 1 1 6 13 48.50 1.40 1 -1 -6 -13 53.40 1.40 1 1 6 14 1.60 0.30 1 -1 -6 -14 1.70 0.40 1 1 6 15 31.90 1.20 1 -1 -6 -15 29.50 1.00 1 1 6 16 12.40 0.60 1 -1 -6 -16 10.80 0.60 1 1 6 17 1.20 0.30 1 -1 -6 -17 1.40 0.40 1 1 6 18 1.00 0.30 1 -1 -6 -18 1.80 0.40 1 1 6 19 0.70 0.30 1 -1 -6 -19 1.80 0.60 1 1 6 20 0.70 0.50 1 -1 -6 -20 1.20 0.70 1 1 6 21 1.50 0.60 1 -1 -6 -21 1.70 0.60 1 1 6 22 2.50 0.70 1 -1 -6 -22 5.80 0.70 1 1 6 23 1.30 0.60 1 -1 -6 -23 1.40 0.60 1 1 6 24 0.40 0.60 1 -1 -6 -24 1.70 0.70 1 1 7 0 193.30 2.50 1 1 7 1 26.80 0.40 1 -1 -7 -1 25.30 0.50 1 1 7 2 50.30 0.70 1 -1 -7 -2 48.70 1.00 1 1 7 3 26.10 0.50 1 -1 -7 -3 26.40 0.60 1 1 7 4 161.20 2.30 1 -1 -7 -4 165.20 2.30 1 1 7 5 46.80 0.80 1 -1 -7 -5 49.60 0.90 1 1 7 6 33.20 0.70 1 -1 -7 -6 32.90 0.70 1 1 7 7 66.10 1.60 1 -1 -7 -7 67.40 1.10 1 1 7 8 50.90 1.10 1 -1 -7 -8 51.60 1.00 1 1 7 9 19.20 0.40 1 -1 -7 -9 20.10 0.40 1 1 7 10 6.10 0.30 1 -1 -7 -10 6.10 0.20 1 1 7 11 93.80 2.40 1 -1 -7 -11 82.10 1.40 1 1 7 12 4.20 0.30 1 -1 -7 -12 4.50 0.30 1 1 7 13 3.10 0.30 1 -1 -7 -13 3.00 0.20 1 1 7 14 33.20 1.20 1 -1 -7 -14 37.50 1.30 1 1 7 15 6.30 0.60 1 -1 -7 -15 5.20 0.60 1 1 7 16 93.50 2.50 1 -1 -7 -16 91.00 2.30 1 1 7 17 1.50 0.40 1 -1 -7 -17 2.40 0.60 1 1 7 18 0.40 0.30 1 -1 -7 -18 1.70 0.60 1 1 7 19 6.80 0.40 1 -1 -7 -19 5.40 0.70 1 1 7 20 18.70 1.60 1 -1 -7 -20 16.30 1.00 1 1 7 21 0.30 0.50 1 -1 -7 -21 1.40 0.50 1 1 7 22 2.30 0.60 1 -1 -7 -22 1.10 0.60 1 1 7 23 0.40 0.60 1 -1 -7 -23 0.60 0.50 1 1 7 24 -0.30 0.80 1 -1 -7 -24 0.50 0.70 1 1 8 0 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24.40 0.80 1 4 4 1 4.70 0.40 1 -4 -4 -1 4.00 0.50 1 4 4 2 34.50 1.00 1 -4 -4 -2 34.50 1.30 1 4 4 3 9.30 0.50 1 -4 -4 -3 7.30 1.10 1 4 4 4 5.60 0.50 1 -4 -4 -4 6.20 0.70 1 4 4 5 29.10 1.10 1 -4 -4 -5 29.80 1.00 1 4 4 6 31.50 1.20 1 -4 -4 -6 27.10 1.20 1 4 4 7 74.70 2.30 1 -4 -4 -7 76.00 2.30 1 4 4 8 2.00 0.60 1 -4 -4 -8 -0.70 0.50 1 4 4 9 6.30 0.60 1 -4 -4 -9 9.40 0.80 1 4 4 10 3.30 0.60 1 -4 -4 -10 3.70 0.70 1 4 4 11 6.40 0.80 1 -4 -4 -11 7.30 0.50 1 4 4 12 23.80 0.90 1 -4 -4 -12 21.50 0.80 1 4 4 13 7.70 0.60 1 -4 -4 -13 5.80 0.50 1 4 4 14 4.00 0.60 1 -4 -4 -14 3.00 0.50 1 4 4 15 7.40 0.70 1 -4 -4 -15 5.40 0.50 1 4 4 16 -0.20 0.50 1 -4 -4 -16 0.30 0.50 1 4 4 17 1.40 0.50 1 -4 -4 -17 2.20 0.50 1 4 4 18 4.80 0.40 1 -4 -4 -18 4.20 0.60 1 4 4 19 3.80 0.30 1 -4 -4 -19 4.50 0.60 1 4 4 20 -0.10 0.50 1 -4 -4 -20 1.10 0.50 1 4 4 21 4.80 0.70 1 -4 -4 -21 3.70 0.50 1 4 4 22 0.10 0.60 1 -4 -4 -22 0.10 0.40 1 4 4 23 -0.20 0.50 1 -4 -4 -23 0.40 0.70 1 4 5 0 268.70 5.50 1 4 5 1 21.00 0.70 1 -4 -5 -1 24.30 1.10 1 4 5 2 51.70 1.30 1 -4 -5 -2 46.70 2.30 1 4 5 3 131.40 3.60 1 -4 -5 -3 137.60 4.00 1 4 5 4 76.70 1.80 1 -4 -5 -4 85.00 2.60 1 4 5 5 3.40 0.50 1 -4 -5 -5 2.40 0.40 1 4 5 6 42.10 2.20 1 -4 -5 -6 42.90 1.30 1 4 5 7 12.00 0.70 1 -4 -5 -7 15.30 0.90 1 4 5 8 30.30 1.20 1 -4 -5 -8 34.60 1.50 1 4 5 9 12.00 0.90 1 -4 -5 -9 12.50 0.90 1 4 5 10 2.40 0.60 1 -4 -5 -10 2.40 0.40 1 4 5 11 2.40 0.60 1 -4 -5 -11 3.30 0.40 1 4 5 12 1.30 0.50 1 -4 -5 -12 1.40 0.40 1 4 5 13 19.50 1.10 1 -4 -5 -13 14.90 0.90 1 4 5 14 -0.20 0.50 1 -4 -5 -14 1.50 0.40 1 4 5 15 5.00 0.60 1 -4 -5 -15 5.90 0.60 1 4 5 16 12.80 0.80 1 -4 -5 -16 8.60 0.60 1 4 5 17 3.00 0.40 1 -4 -5 -17 2.80 0.50 1 4 5 18 1.30 0.30 1 -4 -5 -18 -0.20 0.40 1 4 5 19 0.60 0.30 1 -4 -5 -19 1.50 0.40 1 4 5 20 4.30 0.60 1 -4 -5 -20 3.10 0.50 1 4 5 21 -0.80 0.50 1 -4 -5 -21 -0.40 0.40 1 4 5 22 1.80 0.60 1 -4 -5 -22 2.60 0.90 1 4 5 23 2.20 0.70 1 -4 -5 -23 1.20 0.90 1 4 6 0 314.10 6.40 1 4 6 1 32.30 1.00 1 -4 -6 -1 32.80 1.10 1 4 6 2 41.50 0.90 1 -4 -6 -2 41.20 1.90 1 4 6 3 38.10 0.90 1 -4 -6 -3 39.10 2.10 1 4 6 4 6.90 0.40 1 -4 -6 -4 9.20 1.00 1 4 6 5 10.20 0.50 1 -4 -6 -5 10.00 0.70 1 4 6 6 11.30 0.70 1 -4 -6 -6 12.90 0.60 1 4 6 7 5.50 0.50 1 -4 -6 -7 4.30 0.60 1 4 6 8 15.60 0.80 1 -4 -6 -8 16.00 1.50 1 4 6 9 4.60 0.50 1 -4 -6 -9 9.20 0.90 1 4 6 10 21.70 1.00 1 -4 -6 -10 22.60 0.80 1 4 6 11 4.90 0.70 1 -4 -6 -11 4.40 0.40 1 4 6 12 20.40 0.90 1 -4 -6 -12 21.30 0.70 1 4 6 13 18.10 0.80 1 -4 -6 -13 20.80 0.80 1 4 6 14 0.40 0.50 1 -4 -6 -14 1.70 0.40 1 4 6 15 5.50 0.50 1 -4 -6 -15 6.80 0.50 1 4 6 16 5.80 0.50 1 -4 -6 -16 3.50 0.50 1 4 6 17 5.40 0.50 1 -4 -6 -17 4.70 0.40 1 4 6 18 8.60 0.50 1 -4 -6 -18 9.00 0.60 1 4 6 19 4.30 0.50 1 -4 -6 -19 2.20 0.50 1 4 6 20 2.90 0.60 1 -4 -6 -20 3.60 0.90 1 4 6 21 3.40 0.60 1 -4 -6 -21 2.00 0.90 1 4 6 22 2.80 0.50 1 -4 -6 -22 0.20 0.60 1 4 6 23 0.90 0.50 1 -4 -6 -23 0.60 0.70 1 4 7 0 0.10 0.30 1 4 7 1 32.10 0.70 1 -4 -7 -1 38.60 1.40 1 4 7 2 16.90 0.50 1 -4 -7 -2 16.10 0.80 1 4 7 3 7.50 0.40 1 -4 -7 -3 7.00 1.00 1 4 7 4 24.80 0.70 1 -4 -7 -4 30.20 1.20 1 4 7 5 24.50 0.90 1 -4 -7 -5 31.80 1.30 1 4 7 6 28.90 1.10 1 -4 -7 -6 30.10 1.20 1 4 7 7 12.40 0.70 1 -4 -7 -7 13.80 0.70 1 4 7 8 3.20 0.50 1 -4 -7 -8 1.60 0.70 1 4 7 9 3.10 0.50 1 -4 -7 -9 2.30 0.30 1 4 7 10 20.50 1.40 1 -4 -7 -10 21.20 1.10 1 4 7 11 6.20 0.60 1 -4 -7 -11 5.40 0.40 1 4 7 12 20.50 0.90 1 -4 -7 -12 19.40 0.70 1 4 7 13 4.00 0.50 1 -4 -7 -13 6.00 0.50 1 4 7 14 0.30 0.50 1 -4 -7 -14 0.70 0.40 1 4 7 15 1.90 0.40 1 -4 -7 -15 1.40 0.30 1 4 7 16 10.00 0.60 1 -4 -7 -16 9.70 0.60 1 4 7 17 7.50 0.50 1 -4 -7 -17 7.10 0.50 1 4 7 18 1.60 0.40 1 -4 -7 -18 0.60 0.30 1 4 7 19 1.00 0.40 1 -4 -7 -19 -0.40 0.80 1 4 7 20 3.90 0.70 1 -4 -7 -20 2.80 0.90 1 4 7 21 0.60 0.50 1 -4 -7 -21 0.80 0.80 1 4 7 22 3.00 0.60 1 -4 -7 -22 2.00 0.90 1 4 8 0 6.00 0.40 1 4 8 1 13.70 0.40 1 -4 -8 -1 14.80 0.50 1 4 8 2 36.60 0.80 1 -4 -8 -2 35.40 1.30 1 4 8 3 2.00 0.30 1 -4 -8 -3 3.30 0.80 1 4 8 4 3.00 0.40 1 -4 -8 -4 2.50 0.50 1 4 8 5 126.20 2.90 1 -4 -8 -5 133.10 3.70 1 4 8 6 16.20 0.60 1 -4 -8 -6 16.60 1.00 1 4 8 7 33.60 1.20 1 -4 -8 -7 34.30 1.10 1 4 8 8 2.90 0.40 1 -4 -8 -8 2.60 0.40 1 4 8 9 1.40 0.50 1 -4 -8 -9 0.70 0.30 1 4 8 10 4.20 0.60 1 -4 -8 -10 3.50 0.30 1 4 8 11 3.00 0.50 1 -4 -8 -11 2.80 0.30 1 4 8 12 5.80 0.60 1 -4 -8 -12 7.90 0.40 1 4 8 13 5.40 0.50 1 -4 -8 -13 4.90 0.50 1 4 8 14 13.30 0.60 1 -4 -8 -14 13.70 0.60 1 4 8 15 8.20 0.50 1 -4 -8 -15 8.30 0.50 1 4 8 16 7.30 0.50 1 -4 -8 -16 4.90 0.50 1 4 8 17 10.70 0.50 1 -4 -8 -17 11.60 1.10 1 4 8 18 1.00 0.40 1 -4 -8 -18 -0.50 0.60 1 4 8 19 4.30 0.50 1 -4 -8 -19 2.50 0.80 1 4 8 20 -0.50 0.50 1 -4 -8 -20 1.70 0.70 1 4 8 21 2.80 0.70 1 -4 -8 -21 3.80 0.80 1 4 8 22 1.30 0.50 1 -4 -8 -22 -0.30 0.60 1 4 9 0 0.20 0.20 1 4 9 1 11.80 0.40 1 -4 -9 -1 12.70 0.50 1 4 9 2 5.60 0.30 1 -4 -9 -2 6.70 0.40 1 4 9 3 2.10 0.30 1 -4 -9 -3 1.80 0.30 1 4 9 4 5.30 0.30 1 -4 -9 -4 4.60 0.40 1 4 9 5 5.80 0.40 1 -4 -9 -5 4.20 1.00 1 4 9 6 25.40 0.80 1 -4 -9 -6 25.20 1.20 1 4 9 7 1.20 0.40 1 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10 9 23.40 1.00 1 -4 -10 -9 21.60 0.60 1 4 10 10 5.00 0.50 1 -4 -10 -10 3.70 0.20 1 4 10 11 26.00 1.20 1 -4 -10 -11 20.10 0.60 1 4 10 12 11.10 0.50 1 -4 -10 -12 8.50 0.40 1 4 10 13 6.30 0.40 1 -4 -10 -13 6.10 0.80 1 4 10 14 9.00 0.50 1 -4 -10 -14 9.40 0.90 1 4 10 15 11.40 0.60 1 -4 -10 -15 10.50 0.50 1 4 10 16 14.10 0.60 1 -4 -10 -16 9.20 0.90 1 4 10 17 2.00 0.40 1 -4 -10 -17 -0.20 0.60 1 4 10 18 4.20 0.50 1 -4 -10 -18 5.00 0.70 1 4 10 19 2.30 0.40 1 -4 -10 -19 0.80 0.60 1 4 10 20 0.90 0.80 1 -4 -10 -20 0.30 0.60 1 4 10 21 3.60 0.90 1 -4 -10 -21 4.10 0.90 1 4 11 0 10.00 0.40 1 4 11 1 22.60 0.60 1 -4 -11 -1 21.90 0.70 1 4 11 2 0.40 0.20 1 -4 -11 -2 0.40 0.30 1 4 11 3 9.00 0.40 1 -4 -11 -3 8.60 0.40 1 4 11 4 9.30 0.40 1 -4 -11 -4 9.30 0.50 1 4 11 5 12.50 0.50 1 -4 -11 -5 10.90 0.50 1 4 11 6 5.70 0.40 1 -4 -11 -6 4.70 0.20 1 4 11 7 21.30 0.70 1 -4 -11 -7 20.40 1.00 1 4 11 8 5.80 0.40 1 -4 -11 -8 6.60 0.70 1 4 11 9 26.50 1.00 1 -4 -11 -9 24.60 1.20 1 4 11 10 38.00 1.10 1 -4 -11 -10 36.30 1.50 1 4 11 11 2.50 0.40 1 -4 -11 -11 2.90 0.60 1 4 11 12 10.50 0.50 1 -4 -11 -12 9.50 0.90 1 4 11 13 12.30 0.60 1 -4 -11 -13 9.40 0.80 1 4 11 14 3.50 0.30 1 -4 -11 -14 4.80 0.40 1 4 11 15 2.10 0.40 1 -4 -11 -15 3.40 0.70 1 4 11 16 -0.10 0.40 1 -4 -11 -16 1.60 0.80 1 4 11 17 0.50 0.40 1 -4 -11 -17 2.70 0.80 1 4 11 18 3.90 0.60 1 -4 -11 -18 3.60 0.80 1 4 11 19 4.40 0.60 1 -4 -11 -19 4.60 0.80 1 4 11 20 3.30 0.80 1 -4 -11 -20 2.70 0.90 1 4 11 21 1.10 0.70 1 -4 -11 -21 -0.10 0.80 1 4 12 0 25.80 0.80 1 4 12 1 8.90 0.30 1 -4 -12 -1 9.10 0.50 1 4 12 2 10.00 0.40 1 -4 -12 -2 9.30 0.50 1 4 12 3 4.80 0.30 1 -4 -12 -3 2.80 0.30 1 4 12 4 21.90 0.60 1 -4 -12 -4 17.30 0.70 1 4 12 5 10.40 0.40 1 -4 -12 -5 14.70 1.50 1 4 12 6 10.80 0.50 1 -4 -12 -6 14.10 1.40 1 4 12 7 30.50 0.80 1 -4 -12 -7 30.00 1.90 1 4 12 8 25.60 0.70 1 -4 -12 -8 26.60 1.30 1 4 12 9 3.50 0.40 1 -4 -12 -9 3.50 0.70 1 4 12 10 8.90 0.50 1 -4 -12 -10 7.80 0.80 1 4 12 11 4.10 0.40 1 -4 -12 -11 4.30 0.80 1 4 12 12 6.40 0.40 1 -4 -12 -12 4.60 0.70 1 4 12 13 22.50 0.90 1 -4 -12 -13 23.50 0.80 1 4 12 14 2.10 0.40 1 -4 -12 -14 2.90 0.30 1 4 12 15 4.70 0.60 1 -4 -12 -15 3.10 0.70 1 4 12 16 1.80 0.50 1 -4 -12 -16 -0.50 0.70 1 4 12 17 2.10 0.40 1 -4 -12 -17 2.10 0.80 1 4 12 18 0.20 0.40 1 -4 -12 -18 1.40 0.70 1 4 12 19 2.90 0.60 1 -4 -12 -19 1.30 0.80 1 4 12 20 1.30 0.50 1 -4 -12 -20 0.70 0.60 1 4 13 0 4.50 0.30 1 4 13 1 12.20 0.40 1 -4 -13 -1 9.90 0.50 1 4 13 2 25.80 0.70 1 -4 -13 -2 23.10 1.00 1 4 13 3 29.40 0.80 1 -4 -13 -3 27.90 0.90 1 4 13 4 7.70 0.40 1 -4 -13 -4 6.70 1.00 1 4 13 5 18.80 0.50 1 -4 -13 -5 23.70 1.50 1 4 13 6 21.60 0.70 1 -4 -13 -6 26.60 1.60 1 4 13 7 0.50 0.30 1 -4 -13 -7 0.60 0.90 1 4 13 8 1.40 0.30 1 -4 -13 -8 3.00 0.90 1 4 13 9 22.20 0.80 1 -4 -13 -9 23.40 0.80 1 4 13 10 11.00 0.50 1 -4 -13 -10 13.90 0.70 1 4 13 11 4.00 0.50 1 -4 -13 -11 4.50 0.40 1 4 13 12 10.30 0.60 1 -4 -13 -12 11.20 0.60 1 4 13 13 6.80 0.60 1 -4 -13 -13 6.80 0.50 1 4 13 14 8.10 0.60 1 -4 -13 -14 6.30 0.50 1 4 13 15 3.90 0.60 1 -4 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2.30 0.60 1 -5 -3 -3 3.10 0.60 1 5 3 4 21.10 1.10 1 -5 -3 -4 22.20 1.10 1 5 3 5 15.00 1.00 1 -5 -3 -5 18.60 1.00 1 5 3 6 4.00 0.50 1 -5 -3 -6 3.00 0.70 1 5 3 7 17.90 0.90 1 -5 -3 -7 16.40 1.00 1 5 3 8 22.60 1.10 1 -5 -3 -8 21.70 1.00 1 5 3 9 4.10 0.60 1 -5 -3 -9 3.40 0.70 1 5 3 10 4.20 0.60 1 -5 -3 -10 5.50 0.80 1 5 3 11 4.20 0.80 1 -5 -3 -11 4.80 0.80 1 5 3 12 21.20 1.50 1 -5 -3 -12 23.30 1.20 1 5 3 13 35.50 1.40 1 -5 -3 -13 35.50 1.50 1 5 3 14 7.80 0.70 1 -5 -3 -14 5.80 0.60 1 5 3 15 0.60 0.50 1 -5 -3 -15 0.70 0.40 1 5 3 16 7.50 0.70 1 -5 -3 -16 6.60 0.60 1 5 3 17 0.80 0.60 1 -5 -3 -17 0.80 0.50 1 5 3 18 4.40 0.70 1 -5 -3 -18 6.50 0.60 1 5 3 19 11.20 0.80 1 -5 -3 -19 10.20 0.70 1 5 3 20 3.80 0.70 1 -5 -3 -20 4.10 0.60 1 5 3 21 0.40 0.40 1 -5 -3 -21 3.00 0.50 1 5 3 22 4.40 0.60 1 -5 -3 -22 3.30 0.50 1 5 4 0 10.20 1.00 1 5 4 1 4.10 0.50 1 -5 -4 -1 2.40 0.90 1 5 4 2 15.40 0.70 1 -5 -4 -2 15.80 1.30 1 5 4 3 8.70 0.60 1 -5 -4 -3 10.00 0.90 1 5 4 4 13.90 0.90 1 -5 -4 -4 15.60 1.00 1 5 4 5 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1.90 1.10 1 -5 -22 -1 -2.20 0.90 1 6 0 0 28.80 2.70 1 6 0 1 131.30 3.80 1 6 0 2 1.80 0.40 1 6 0 3 6.70 0.80 1 6 0 4 33.80 1.50 1 6 0 5 14.40 1.00 1 6 0 6 23.20 1.20 1 6 0 7 6.80 0.80 1 6 0 8 3.20 0.70 1 6 0 9 13.70 0.80 1 6 0 10 28.00 1.30 1 6 0 11 22.70 1.20 1 6 0 12 4.10 0.70 1 6 0 13 -0.20 0.60 1 6 0 14 0.10 0.70 1 6 0 15 3.80 0.50 1 6 0 16 3.80 0.60 1 6 0 17 0.90 0.50 1 6 0 18 5.90 0.70 1 6 0 19 0.70 0.60 1 6 0 20 4.50 0.60 1 6 0 21 0.30 0.50 1 6 1 1 56.40 1.90 1 -6 -1 -1 45.70 1.70 1 6 1 2 9.30 0.70 1 -6 -1 -2 11.30 1.20 1 6 1 3 6.20 0.70 1 -6 -1 -3 4.70 0.70 1 6 1 4 23.80 1.10 1 -6 -1 -4 25.20 1.30 1 6 1 5 26.70 1.30 1 -6 -1 -5 28.60 1.30 1 6 1 6 30.10 1.40 1 -6 -1 -6 26.00 1.20 1 6 1 7 18.50 1.10 1 -6 -1 -7 17.60 1.10 1 6 1 8 4.70 0.80 1 -6 -1 -8 2.00 0.80 1 6 1 9 2.90 0.70 1 -6 -1 -9 3.90 0.90 1 6 1 10 33.60 1.40 1 -6 -1 -10 32.90 1.50 1 6 1 11 7.20 0.80 1 -6 -1 -11 13.40 1.40 1 6 1 12 4.60 0.80 1 -6 -1 -12 4.20 0.80 1 6 1 13 20.20 1.10 1 -6 -1 -13 18.20 1.10 1 6 1 14 15.90 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-9 -7 -7 -0.50 1.10 1 9 7 8 0.50 0.60 1 -9 -7 -8 -1.90 1.00 1 9 7 9 1.20 0.70 1 -9 -7 -9 -0.70 0.80 1 9 7 10 0.50 0.60 1 -9 -7 -10 1.60 1.10 1 9 7 11 1.20 0.60 1 -9 -7 -11 -0.40 0.60 1 9 7 12 -0.20 0.70 1 -9 -7 -12 -0.60 0.90 1 9 7 13 0.90 0.80 1 -9 -7 -13 0.90 0.80 1 9 8 0 2.00 0.70 1 9 8 1 0.40 0.70 1 -9 -8 -1 0.00 0.70 1 9 8 2 3.10 0.80 1 -9 -8 -2 1.60 0.70 1 9 8 3 2.20 0.70 1 -9 -8 -3 3.10 0.80 1 9 8 4 3.60 0.70 1 -9 -8 -4 0.80 0.70 1 9 8 5 1.00 0.50 1 -9 -8 -5 1.00 0.70 1 9 8 6 2.40 0.60 1 -9 -8 -6 1.20 1.10 1 9 8 7 1.50 0.60 1 -9 -8 -7 4.50 1.20 1 9 8 8 -0.50 0.60 1 -9 -8 -8 -0.60 1.10 1 9 8 9 0.80 0.50 1 -9 -8 -9 0.30 1.10 1 9 8 10 1.60 0.60 1 -9 -8 -10 1.90 1.20 1 9 8 11 2.60 0.60 1 -9 -8 -11 2.30 1.20 1 9 8 12 -1.50 0.70 1 -9 -8 -12 0.50 0.60 1 9 9 0 2.70 0.70 1 9 9 1 2.70 0.70 1 -9 -9 -1 1.60 0.50 1 9 9 2 0.50 0.60 1 -9 -9 -2 1.20 0.70 1 9 9 3 4.50 0.70 1 -9 -9 -3 2.50 0.70 1 9 9 4 1.10 0.70 1 -9 -9 -4 0.90 0.80 1 9 9 5 0.40 0.60 1 -9 -9 -5 0.30 0.60 1 9 9 6 -0.10 0.60 1 -9 -9 -6 -1.00 1.10 1 9 9 7 2.30 0.50 1 -9 -9 -7 -0.30 1.10 1 9 9 8 0.60 0.60 1 -9 -9 -8 1.80 1.10 1 9 9 9 0.30 0.50 1 -9 -9 -9 1.60 1.20 1 9 9 10 2.80 0.80 1 -9 -9 -10 4.30 1.10 1 9 9 11 0.70 0.50 1 -9 -9 -11 1.00 1.30 1 9 9 12 7.10 0.80 1 -9 -9 -12 7.50 1.50 1 9 10 0 0.10 0.60 1 9 10 1 0.70 0.70 1 -9 -10 -1 0.60 0.70 1 9 10 2 0.90 0.60 1 -9 -10 -2 2.00 0.70 1 9 10 3 1.00 0.70 1 -9 -10 -3 1.30 0.70 1 9 10 4 1.40 0.60 1 -9 -10 -4 1.90 0.70 1 9 10 5 -0.10 0.60 1 -9 -10 -5 1.40 0.60 1 9 10 6 0.50 0.50 1 -9 -10 -6 1.20 1.10 1 9 10 7 1.40 0.60 1 -9 -10 -7 1.80 0.80 1 9 10 8 0.30 0.50 1 -9 -10 -8 -0.30 1.10 1 9 10 9 3.60 0.60 1 -9 -10 -9 1.40 1.40 1 9 10 10 0.20 0.60 1 -9 -10 -10 0.50 1.00 1 9 10 11 2.50 0.90 1 -9 -10 -11 0.10 1.10 1 9 11 0 0.30 0.70 1 9 11 1 -1.80 0.60 1 -9 -11 -1 1.80 0.70 1 9 11 2 -0.40 0.50 1 -9 -11 -2 -0.20 0.70 1 9 11 3 1.70 0.60 1 -9 -11 -3 1.60 0.70 1 9 11 4 1.70 0.70 1 -9 -11 -4 1.50 0.50 1 9 11 5 4.00 0.80 1 -9 -11 -5 -0.10 1.00 1 9 11 6 -0.30 0.50 1 -9 -11 -6 -0.50 1.00 1 9 11 7 1.50 0.60 1 -9 -11 -7 2.20 0.80 1 9 11 8 -0.10 0.80 1 -9 -11 -8 1.00 1.10 1 9 11 9 1.70 1.10 1 -9 -11 -9 1.90 1.10 1 9 11 10 0.00 0.70 1 -9 -11 -10 -1.00 0.90 1 9 12 0 3.70 0.70 1 9 12 1 5.10 0.70 1 -9 -12 -1 6.60 0.70 1 9 12 2 2.40 0.70 1 -9 -12 -2 1.80 0.80 1 9 12 3 2.20 0.60 1 -9 -12 -3 2.90 0.70 1 9 12 4 0.90 0.60 1 -9 -12 -4 -0.60 0.60 1 9 12 5 0.70 1.20 1 -9 -12 -5 0.70 0.80 1 9 12 6 2.20 0.80 1 -9 -12 -6 4.40 0.90 1 9 12 7 4.20 0.90 1 -9 -12 -7 3.10 1.20 1 9 12 8 3.60 0.80 1 -9 -12 -8 -0.80 1.20 1 9 13 0 -1.20 0.60 1 9 13 1 0.20 1.20 1 -9 -13 -1 2.10 0.70 1 9 13 2 6.80 1.40 1 -9 -13 -2 4.60 0.70 1 9 13 3 1.00 1.30 1 -9 -13 -3 5.70 0.80 1 9 13 4 -0.10 1.20 1 -9 -13 -4 1.00 0.70 1 9 13 5 -1.60 1.10 1 -9 -13 -5 1.10 0.70 1 9 13 6 -0.30 0.70 1 -9 -13 -6 -1.00 1.00 1 9 13 7 0.90 0.70 1 -9 -13 -7 -1.40 1.10 1 9 14 0 0.60 1.10 1 9 14 1 2.00 1.20 1 -9 -14 -1 -0.40 1.10 1 9 14 2 -0.60 1.10 1 -9 -14 -2 2.00 0.70 1 9 14 3 1.10 1.20 1 -9 -14 -3 1.70 1.20 1 9 14 4 3.00 1.30 1 -9 -14 -4 1.30 0.60 1 10 0 0 20.00 1.80 1 10 0 1 1.50 0.80 1 10 0 2 0.60 0.70 1 10 0 3 0.00 0.80 1 10 0 4 -1.60 0.70 1 10 0 5 -1.20 0.70 1 10 0 6 -0.90 0.80 1 10 0 7 3.90 0.80 1 10 0 8 -0.90 0.80 1 10 0 9 1.50 0.80 1 10 0 10 2.90 1.00 1 10 0 11 2.80 0.90 1 10 1 0 3.40 0.80 1 10 1 1 4.20 0.80 1 -10 -1 -1 3.80 0.70 1 10 1 2 10.10 1.10 1 -10 -1 -2 5.80 0.80 1 10 1 3 -0.70 0.80 1 -10 -1 -3 1.50 0.60 1 10 1 4 1.10 0.80 1 -10 -1 -4 0.00 0.80 1 10 1 5 0.70 0.80 1 -10 -1 -5 0.80 0.60 1 10 1 6 0.00 0.80 1 -10 -1 -6 -1.10 0.90 1 10 1 7 0.90 0.70 1 -10 -1 -7 -0.10 0.60 1 10 1 8 2.30 0.60 1 -10 -1 -8 -0.40 0.80 1 10 1 9 1.00 0.90 1 -10 -1 -9 2.00 0.90 1 10 1 10 4.40 0.90 1 -10 -1 -10 5.30 0.90 1 10 1 11 -1.20 0.70 1 -10 -1 -11 1.50 0.80 1 10 2 0 12.80 1.00 1 10 2 1 -0.10 0.70 1 -10 -2 -1 -1.10 0.70 1 10 2 2 1.30 0.80 1 -10 -2 -2 2.30 0.60 1 10 2 3 0.70 0.70 1 -10 -2 -3 -0.30 0.80 1 10 2 4 4.10 0.90 1 -10 -2 -4 1.30 0.70 1 10 2 5 2.30 0.70 1 -10 -2 -5 0.60 0.80 1 10 2 6 0.10 0.80 1 -10 -2 -6 2.60 0.80 1 10 2 7 1.90 0.70 1 -10 -2 -7 1.30 0.80 1 10 2 8 3.50 0.70 1 -10 -2 -8 4.70 1.30 1 10 2 9 0.50 0.70 1 -10 -2 -9 -0.50 0.70 1 10 2 10 -0.20 0.70 1 -10 -2 -10 0.90 0.90 1 10 2 11 1.70 0.80 1 -10 -2 -11 0.50 0.80 1 10 3 0 -0.30 0.70 1 10 3 1 2.60 0.80 1 -10 -3 -1 0.00 0.80 1 10 3 2 0.20 0.60 1 -10 -3 -2 -0.60 0.80 1 10 3 3 -0.30 0.70 1 -10 -3 -3 1.50 0.80 1 10 3 4 0.00 0.70 1 -10 -3 -4 -1.40 0.70 1 10 3 5 1.70 1.20 1 -10 -3 -5 0.90 0.60 1 10 3 6 1.50 1.00 1 -10 -3 -6 0.20 1.10 1 10 3 7 1.90 0.80 1 -10 -3 -7 2.40 0.70 1 10 3 8 0.10 0.60 1 -10 -3 -8 0.80 0.70 1 10 3 9 -0.50 0.70 1 -10 -3 -9 2.00 1.20 1 10 3 10 -0.80 0.80 1 -10 -3 -10 1.60 0.80 1 10 3 11 0.80 0.80 1 -10 -3 -11 3.90 1.00 1 10 4 0 1.50 0.70 1 10 4 1 1.00 0.70 1 -10 -4 -1 1.00 0.60 1 10 4 2 0.30 0.70 1 -10 -4 -2 -2.20 0.70 1 10 4 3 1.40 0.70 1 -10 -4 -3 3.00 0.70 1 10 4 4 1.80 1.10 1 -10 -4 -4 -0.70 0.70 1 10 4 5 0.20 0.80 1 -10 -4 -5 2.00 0.70 1 10 4 6 1.40 1.00 1 -10 -4 -6 0.80 0.90 1 10 4 7 0.50 0.60 1 -10 -4 -7 -0.50 0.60 1 10 4 8 2.50 0.60 1 -10 -4 -8 4.80 1.20 1 10 4 9 0.00 0.60 1 -10 -4 -9 0.90 0.80 1 10 4 10 2.00 0.80 1 -10 -4 -10 -0.20 1.20 1 10 5 0 1.10 0.80 1 10 5 1 2.70 0.80 1 -10 -5 -1 1.60 0.70 1 10 5 2 0.00 0.80 1 -10 -5 -2 -1.60 0.70 1 10 5 3 -0.90 0.60 1 -10 -5 -3 -0.10 0.60 1 10 5 4 1.70 0.90 1 -10 -5 -4 0.00 0.70 1 10 5 5 0.10 1.10 1 -10 -5 -5 3.00 0.90 1 10 5 6 2.40 0.70 1 -10 -5 -6 3.20 1.00 1 10 5 7 0.90 0.70 1 -10 -5 -7 0.30 0.70 1 10 5 8 1.50 0.70 1 -10 -5 -8 2.60 0.90 1 10 5 9 0.10 0.60 1 -10 -5 -9 -1.20 1.00 1 10 5 10 1.00 0.70 1 -10 -5 -10 2.40 0.80 1 10 6 0 0.10 0.70 1 10 6 1 1.90 0.70 1 -10 -6 -1 1.30 0.60 1 10 6 2 0.20 0.60 1 -10 -6 -2 0.00 0.70 1 10 6 3 0.70 0.70 1 -10 -6 -3 2.60 0.90 1 10 6 4 1.50 0.60 1 -10 -6 -4 1.70 0.70 1 10 6 5 1.10 0.70 1 -10 -6 -5 -0.60 0.70 1 10 6 6 0.90 0.70 1 -10 -6 -6 0.60 0.70 1 10 6 7 0.20 0.50 1 -10 -6 -7 0.60 0.80 1 10 6 8 3.30 0.70 1 -10 -6 -8 4.70 1.30 1 10 6 9 1.40 0.70 1 -10 -6 -9 3.10 1.30 1 10 7 0 1.10 0.70 1 10 7 1 3.60 0.80 1 -10 -7 -1 1.30 0.60 1 10 7 2 0.50 0.70 1 -10 -7 -2 -0.70 0.70 1 10 7 3 0.60 0.70 1 -10 -7 -3 3.20 1.10 1 10 7 4 1.50 0.80 1 -10 -7 -4 -1.30 0.60 1 10 7 5 1.30 0.70 1 -10 -7 -5 -0.40 0.70 1 10 7 6 2.10 0.80 1 -10 -7 -6 2.70 0.80 1 10 7 7 1.60 0.60 1 -10 -7 -7 -1.10 0.80 1 10 7 8 1.20 0.60 1 -10 -7 -8 1.80 1.30 1 10 8 0 -0.80 0.70 1 10 8 1 1.90 0.80 1 -10 -8 -1 2.40 0.80 1 10 8 2 -1.00 0.80 1 -10 -8 -2 -0.50 0.70 1 10 8 3 1.70 0.80 1 -10 -8 -3 1.00 0.70 1 10 8 4 0.80 0.70 1 -10 -8 -4 0.50 0.50 1 10 8 5 -0.60 0.70 1 -10 -8 -5 0.70 1.10 1 10 8 6 -0.30 0.70 1 -10 -8 -6 -0.10 0.80 1 10 8 7 3.50 0.70 1 -10 -8 -7 2.50 0.70 1 10 9 0 -0.30 0.70 1 10 9 1 1.50 0.60 1 -10 -9 -1 0.30 0.70 1 10 9 2 -0.40 0.70 1 -10 -9 -2 0.00 0.70 1 10 9 3 -0.40 0.70 1 -10 -9 -3 1.40 0.80 1 10 9 4 2.70 0.70 1 -10 -9 -4 -0.30 0.60 1 10 9 5 1.10 0.80 1 -10 -9 -5 0.40 0.70 1 10 9 6 2.60 0.70 1 -10 -9 -6 2.10 0.90 1 10 10 0 -0.20 0.60 1 10 10 1 0.70 0.70 1 -10 -10 -1 0.60 0.80 1 10 10 2 1.00 0.80 1 -10 -10 -2 -0.20 0.70 1 10 10 3 0.20 0.70 1 -10 -10 -3 -0.70 0.60 1 10 10 4 0.60 0.70 1 -10 -10 -4 -0.80 0.70 1 10 11 0 1.40 0.70 1 10 11 1 1.60 0.80 1 -10 -11 -1 2.00 0.70 1 11 0 0 1.70 1.20 1 11 0 1 1.30 0.80 1 11 0 2 3.50 0.90 1 11 0 3 4.60 0.80 1 11 0 4 3.50 0.90 1 11 1 0 12.70 0.90 1 11 1 1 2.50 0.90 1 -11 -1 -1 -0.30 0.70 1 11 1 2 2.30 0.90 1 -11 -1 -2 2.20 0.90 1 11 1 3 -1.30 0.70 1 -11 -1 -3 0.50 0.80 1 11 1 4 2.20 0.80 1 -11 -1 -4 0.80 0.80 1 11 2 0 4.00 1.40 1 11 2 1 0.60 0.80 1 -11 -2 -1 -0.90 0.90 1 11 2 2 -0.50 0.80 1 -11 -2 -2 0.90 0.70 1 11 2 3 0.40 0.70 1 -11 -2 -3 1.10 0.80 1 11 2 4 0.20 0.80 1 -11 -2 -4 -0.80 0.80 1 11 3 0 0.50 0.90 1 11 3 1 2.50 0.80 1 -11 -3 -1 -0.10 0.80 1 11 3 2 0.70 0.60 1 -11 -3 -2 0.80 0.60 1 11 3 3 0.90 0.60 1 -11 -3 -3 0.60 0.60 1 11 4 0 2.80 0.70 1 11 4 1 3.70 0.90 1 -11 -4 -1 4.20 0.80 1 11 4 2 1.50 0.70 1 -11 -4 -2 2.30 0.90 1 0 0 0 ; _shelx_hkl_checksum 11058 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N1 0.8336(2) 0.7099(7) 0.6285(3) 0.0340(13) Uani d . . . 1.0 . . N N3 0.9956(2) 0.6991(7) 0.5652(3) 0.0353(13) Uani d . . . 1.0 . . C C1 0.9333(3) 0.7209(8) 0.6984(3) 0.0370(16) Uani d . . . 1.0 . . C C2 0.9046(4) 0.7205(11) 0.7698(3) 0.048(2) Uani d . . . 1.0 . . H H2A 0.885 0.8188 0.7807 0.058 Uiso calc U . R 1.0 . . H H2B 0.8712 0.6415 0.7744 0.058 Uiso calc U . R 1.0 . . C C3 0.9623(4) 0.6885(11) 0.8156(4) 0.051(2) Uani d . . . 1.0 . . H H3A 0.9554 0.7316 0.8613 0.061 Uiso calc U . R 1.0 . . H H3B 0.9697 0.5793 0.8199 0.061 Uiso calc U . R 1.0 . . C C4 1.0179(4) 0.7628(10) 0.7808(3) 0.048(2) Uani d . . . 1.0 . . H H4A 1.0596 0.7188 0.7956 0.058 Uiso calc U . R 1.0 . . H H4B 1.0184 0.8718 0.7901 0.058 Uiso calc U . R 1.0 . . C C5 1.0058(3) 0.7322(9) 0.7056(4) 0.0397(17) Uani d . . . 1.0 . . H H5A 1.023 0.815 0.6774 0.048 Uiso calc U . R 1.0 . . H H5B 1.0269 0.6374 0.6915 0.048 Uiso calc U . R 1.0 . . C C7 0.9030(3) 0.7121(8) 0.6378(3) 0.0342(15) Uani d . . . 1.0 . . C C8 0.9335(3) 0.7016(8) 0.5687(3) 0.0327(15) Uani d . . . 1.0 . . C C9 0.8149(3) 0.6981(8) 0.5635(3) 0.0321(14) Uani d . . . 1.0 . . C C11 0.7890(3) 0.7477(8) 0.6828(3) 0.0341(15) Uani d . . . 1.0 . . C C12 0.7809(4) 0.8990(9) 0.6994(4) 0.0429(18) Uani d . . . 1.0 . . C C13 0.7398(4) 0.9326(11) 0.7527(4) 0.053(2) Uani d . . . 1.0 . . H H13 0.7334 1.0344 0.7654 0.063 Uiso calc U . R 1.0 . . C C14 0.7083(4) 0.8229(13) 0.7872(4) 0.061(2) Uani d . . . 1.0 . . H H14 0.6803 0.8493 0.8236 0.073 Uiso calc U . R 1.0 . . C C15 0.7161(4) 0.6750(12) 0.7706(4) 0.056(2) Uani d . . . 1.0 . . H H15 0.694 0.6003 0.796 0.067 Uiso calc U . R 1.0 . . C C16 0.7567(4) 0.6312(10) 0.7158(4) 0.0454(19) Uani d . . . 1.0 . . C C17 0.8194(4) 1.0193(10) 0.6649(4) 0.055(2) Uani d . . . 1.0 . . H H17A 0.8263 0.9918 0.6173 0.083 Uiso calc U . R 1.0 . . H H17B 0.8613 1.0305 0.6876 0.083 Uiso calc U . R 1.0 . . H H17C 0.7956 1.1143 0.6671 0.083 Uiso calc U . R 1.0 . . C C18 0.7657(5) 0.4706(10) 0.6983(5) 0.059(2) Uani d . . . 1.0 . . H H18A 0.7394 0.4459 0.6585 0.088 Uiso calc U . R 1.0 . . H H18B 0.7521 0.4082 0.7367 0.088 Uiso calc U . R 1.0 . . H H18C 0.8115 0.4517 0.6883 0.088 Uiso calc U . R 1.0 . . N N2 0.7510(2) 0.7035(7) 0.5507(3) 0.0335(13) Uani d . . D 1.0 . . H H2 0.721(4) 0.744(9) 0.584(4) 0.04(2) Uiso d . . . 1.0 . . C C21 0.7213(15) 0.7305(19) 0.4842(9) 0.033(4) Uani d U P D 0.67(3) A 1 C C22 0.7179(10) 0.876(2) 0.4593(8) 0.037(4) Uani d U P D 0.67(3) A 1 C C23 0.6880(7) 0.899(2) 0.3969(7) 0.041(3) Uani d U P D 0.67(3) A 1 H H23 0.684 0.9984 0.3798 0.049 Uiso calc U P R 0.67(3) A 1 C C24 0.6642(6) 0.780(2) 0.3596(6) 0.041(3) Uani d U P D 0.67(3) A 1 H H24 0.6455 0.7976 0.3163 0.049 Uiso calc U P R 0.67(3) A 1 C C25 0.6674(7) 0.636(2) 0.3849(7) 0.044(4) Uani d U P D 0.67(3) A 1 H H25 0.6491 0.5554 0.36 0.053 Uiso calc U P R 0.67(3) A 1 C C26 0.6972(9) 0.609(2) 0.4467(8) 0.040(4) Uani d U P D 0.67(3) A 1 C C27 0.7440(13) 1.006(2) 0.4991(13) 0.055(5) Uani d U P D 0.67(3) A 1 H H27A 0.7373 1.0988 0.4735 0.083 Uiso calc U P R 0.67(3) A 1 H H27B 0.7213 1.0123 0.5426 0.083 Uiso calc U P R 0.67(3) A 1 H H27C 0.7904 0.9913 0.5071 0.083 Uiso calc U P R 0.67(3) A 1 C C28 0.6962(10) 0.4488(19) 0.4737(11) 0.059(5) Uani d U P D 0.67(3) A 1 H H28A 0.7187 0.445 0.5174 0.088 Uiso calc U P R 0.67(3) A 1 H H28B 0.6512 0.4161 0.4796 0.088 Uiso calc U P R 0.67(3) A 1 H H28C 0.718 0.3824 0.4414 0.088 Uiso calc U P R 0.67(3) A 1 C C21A 0.723(3) 0.703(3) 0.4827(19) 0.031(9) Uani d U P D 0.33(3) A 2 C C22A 0.713(2) 0.839(3) 0.4507(16) 0.035(8) Uani d U P D 0.33(3) A 2 C C23A 0.6816(16) 0.842(4) 0.3883(13) 0.037(7) Uani d U P D 0.33(3) A 2 H H23A 0.6739 0.9343 0.3655 0.045 Uiso calc U P R 0.33(3) A 2 C C24A 0.6622(14) 0.708(4) 0.3609(13) 0.036(6) Uani d U P D 0.33(3) A 2 H H24A 0.6463 0.7062 0.3157 0.043 Uiso calc U P R 0.33(3) A 2 C C25A 0.6654(16) 0.578(4) 0.3974(14) 0.048(7) Uani d U P D 0.33(3) A 2 H H25A 0.6482 0.4885 0.3781 0.057 Uiso calc U P R 0.33(3) A 2 C C26A 0.6925(17) 0.572(3) 0.4608(15) 0.034(8) Uani d U P D 0.33(3) A 2 C C27A 0.740(2) 0.981(4) 0.4808(18) 0.038(9) Uani d U P D 0.33(3) A 2 H H27D 0.7283 1.0664 0.4519 0.057 Uiso calc U P R 0.33(3) A 2 H H27E 0.7215 0.996 0.5262 0.057 Uiso calc U P R 0.33(3) A 2 H H27F 0.7871 0.9734 0.4841 0.057 Uiso calc U P R 0.33(3) A 2 C C28A 0.690(2) 0.430(4) 0.502(2) 0.068(11) Uani d U P D 0.33(3) A 2 H H28D 0.7117 0.4463 0.5457 0.102 Uiso calc U P R 0.33(3) A 2 H H28E 0.6448 0.4016 0.51 0.102 Uiso calc U P R 0.33(3) A 2 H H28F 0.7121 0.3492 0.4775 0.102 Uiso calc U P R 0.33(3) A 2 C C31 1.0287(3) 0.6985(8) 0.5019(3) 0.0334(15) Uani d . . . 1.0 . . C C32 1.0596(3) 0.5676(9) 0.4795(3) 0.0387(16) Uani d . . . 1.0 . . C C33 1.0937(3) 0.5710(10) 0.4190(4) 0.0474(19) Uani d . . . 1.0 . . H H33 1.1127 0.4813 0.4021 0.057 Uiso calc U . R 1.0 . . C C34 1.1007(3) 0.7035(11) 0.3828(4) 0.049(2) Uani d . . . 1.0 . . H H34 1.1232 0.7043 0.3408 0.059 Uiso calc U . R 1.0 . . C C35 1.0746(3) 0.8335(10) 0.4085(4) 0.0446(19) Uani d . . . 1.0 . . H H35 1.0811 0.9254 0.3851 0.054 Uiso calc U . R 1.0 . . C C36 1.0388(3) 0.8324(9) 0.4683(4) 0.0418(17) Uani d . . . 1.0 . . C C37 1.0586(4) 0.4251(9) 0.5212(4) 0.051(2) Uani d . . . 1.0 . . H H37A 1.102 0.4054 0.5391 0.076 Uiso calc U . R 1.0 . . H H37B 1.0449 0.341 0.4926 0.076 Uiso calc U . R 1.0 . . H H37C 1.028 0.4367 0.5589 0.076 Uiso calc U . R 1.0 . . C C38 1.0128(4) 0.9788(9) 0.4971(4) 0.051(2) Uani d . . . 1.0 . . H H38A 1.03 0.9939 0.5429 0.076 Uiso calc U . R 1.0 . . H H38B 0.9653 0.9746 0.499 0.076 Uiso calc U . R 1.0 . . H H38C 1.0262 1.0623 0.468 0.076 Uiso calc U . R 1.0 . . B B1 0.8755(3) 0.6986(9) 0.5123(4) 0.0315(16) Uani d . . . 1.0 . . H H1 0.875(3) 0.818(8) 0.491(3) 0.034(18) Uiso d . . . 1.0 . . C C41 0.8874(3) 0.5718(8) 0.4536(3) 0.0298(14) Uani d . . . 1.0 . . C C42 0.9017(3) 0.6148(8) 0.3852(3) 0.0336(15) Uani d . . . 1.0 . . C C43 0.9304(3) 0.5193(9) 0.3396(3) 0.0397(17) Uani d . . . 1.0 . . H H43 0.9413 0.5548 0.2956 0.048 Uiso calc U . R 1.0 . . C C45 0.9242(3) 0.3192(9) 0.4199(3) 0.0377(16) Uani d . . . 1.0 . . H H45 0.929 0.2159 0.4307 0.045 Uiso calc U . R 1.0 . . C C46 0.8976(3) 0.4177(8) 0.4668(3) 0.0324(15) Uani d . . . 1.0 . . C C47 0.8836(3) 0.7669(9) 0.3582(3) 0.0389(17) Uani d . . . 1.0 . . F F1 0.9235(2) 0.8772(5) 0.3764(2) 0.0562(12) Uani d . . . 1.0 . . F F2 0.82365(19) 0.8100(6) 0.3761(2) 0.0528(12) Uani d . . . 1.0 . . F F3 0.8827(2) 0.7664(6) 0.28987(19) 0.0547(12) Uani d . . . 1.0 . . C C44 0.9437(3) 0.3736(9) 0.3566(3) 0.0389(17) Uani d . . . 1.0 . . C C48 0.9793(4) 0.2708(10) 0.3098(4) 0.0479(19) Uani d U . . 1.0 . . F F4 0.9865(3) 0.3272(6) 0.2487(2) 0.0713(16) Uani d U . . 1.0 . . F F5 0.9499(3) 0.1411(7) 0.3006(3) 0.092(2) Uani d U . . 1.0 . . F F6 1.0377(3) 0.2372(8) 0.3324(2) 0.086(2) Uani d U . . 1.0 . . C C49 0.8790(3) 0.3454(8) 0.5335(3) 0.0360(15) Uani d . . D 1.0 . . F F7 0.8902(4) 0.2009(7) 0.5362(3) 0.060(3) Uani d U P D 0.775(14) B 1 F F8 0.9081(4) 0.4066(8) 0.5873(3) 0.058(2) Uani d U P D 0.775(14) B 1 F F9 0.8161(3) 0.3615(10) 0.5471(3) 0.065(3) Uani d U P D 0.775(14) B 1 F F7A 0.9277(11) 0.263(4) 0.5592(12) 0.074(9) Uani d U P D 0.225(14) B 2 F F8A 0.8552(19) 0.426(3) 0.5821(13) 0.092(11) Uani d U P D 0.225(14) B 2 F F9A 0.8330(13) 0.240(3) 0.5217(13) 0.081(10) Uani d U P D 0.225(14) B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.029(3) 0.046(4) 0.027(3) -0.002(3) 0.005(2) 0.001(3) N3 0.027(3) 0.047(4) 0.032(3) 0.001(3) 0.001(2) 0.004(3) C1 0.036(3) 0.045(4) 0.030(3) -0.001(3) 0.001(3) -0.001(3) C2 0.047(4) 0.075(6) 0.022(3) 0.003(4) 0.001(3) -0.003(3) C3 0.058(5) 0.064(5) 0.031(4) 0.002(4) -0.012(3) 0.005(4) C4 0.043(4) 0.066(6) 0.035(4) 0.001(4) -0.011(3) -0.002(4) C5 0.033(3) 0.044(4) 0.042(4) -0.001(3) -0.007(3) 0.001(3) C7 0.029(3) 0.045(4) 0.029(3) -0.003(3) 0.000(3) 0.003(3) C8 0.037(4) 0.035(4) 0.027(3) -0.002(3) 0.001(3) 0.004(3) C9 0.033(3) 0.031(4) 0.032(3) 0.001(3) 0.000(3) 0.001(3) C11 0.028(3) 0.049(4) 0.025(3) -0.001(3) 0.002(2) -0.005(3) C12 0.048(4) 0.047(5) 0.033(4) -0.005(4) -0.001(3) -0.007(3) C13 0.045(4) 0.061(6) 0.052(5) 0.000(4) -0.002(4) -0.020(4) C14 0.045(4) 0.095(8) 0.043(4) -0.002(5) 0.008(4) -0.018(5) C15 0.047(4) 0.080(7) 0.041(4) -0.014(5) 0.014(4) 0.006(4) C16 0.050(4) 0.054(5) 0.033(4) -0.010(4) 0.003(3) -0.006(3) C17 0.063(5) 0.041(5) 0.060(5) -0.007(4) 0.004(4) -0.008(4) C18 0.070(6) 0.049(5) 0.057(5) -0.008(4) 0.012(4) 0.012(4) N2 0.025(3) 0.046(4) 0.029(3) 0.002(3) 0.001(2) -0.001(3) C21 0.024(6) 0.046(7) 0.030(6) 0.005(7) 0.006(4) -0.007(6) C22 0.032(6) 0.037(7) 0.041(6) 0.002(6) 0.005(5) -0.005(6) C23 0.033(5) 0.042(7) 0.047(6) 0.004(6) 0.007(5) 0.010(6) C24 0.037(5) 0.047(8) 0.037(5) -0.001(6) 0.002(4) -0.003(6) C25 0.048(6) 0.043(8) 0.042(6) -0.002(6) -0.003(5) 0.000(6) C26 0.039(6) 0.039(7) 0.042(7) 0.002(6) 0.005(5) -0.002(5) C27 0.057(9) 0.041(8) 0.068(13) -0.003(7) -0.004(9) -0.005(8) C28 0.056(8) 0.051(9) 0.070(11) -0.013(7) -0.010(8) -0.006(8) C21A 0.025(11) 0.036(11) 0.034(11) 0.006(9) 0.001(8) 0.002(8) C22A 0.032(10) 0.035(11) 0.038(10) 0.002(8) 0.002(7) -0.004(8) C23A 0.037(9) 0.038(10) 0.035(9) -0.002(8) -0.002(7) -0.003(8) C24A 0.034(8) 0.038(10) 0.037(9) -0.001(8) 0.000(7) -0.004(8) C25A 0.047(10) 0.048(11) 0.048(10) -0.002(8) 0.001(8) -0.006(8) C26A 0.030(9) 0.035(11) 0.036(10) -0.003(8) -0.001(8) 0.001(8) C27A 0.040(14) 0.052(17) 0.022(12) 0.011(12) 0.014(10) -0.015(11) C28A 0.066(16) 0.046(15) 0.09(2) 0.006(13) -0.002(16) -0.011(14) C31 0.022(3) 0.045(4) 0.033(3) -0.001(3) -0.002(3) 0.002(3) C32 0.031(3) 0.046(5) 0.039(4) -0.001(3) 0.000(3) -0.007(3) C33 0.034(4) 0.062(5) 0.046(4) 0.000(4) -0.004(3) -0.013(4) C34 0.037(4) 0.078(6) 0.032(3) -0.001(4) 0.000(3) -0.004(4) C35 0.040(4) 0.057(5) 0.036(4) -0.001(4) 0.000(3) 0.011(4) C36 0.035(4) 0.045(5) 0.046(4) -0.002(3) -0.003(3) -0.001(4) C37 0.040(4) 0.043(5) 0.068(5) 0.006(3) -0.009(4) -0.001(4) C38 0.051(5) 0.042(5) 0.059(5) 0.005(4) 0.006(4) 0.003(4) B1 0.030(4) 0.036(4) 0.029(4) 0.002(3) 0.003(3) 0.002(3) C41 0.019(3) 0.043(4) 0.028(3) 0.001(3) 0.000(2) 0.001(3) C42 0.033(3) 0.038(4) 0.030(3) 0.002(3) 0.000(3) -0.003(3) C43 0.030(3) 0.055(5) 0.034(3) -0.006(3) 0.000(3) 0.005(3) C45 0.037(4) 0.043(4) 0.033(3) -0.001(3) 0.000(3) 0.002(3) C46 0.030(3) 0.036(4) 0.031(3) -0.003(3) -0.001(3) -0.002(3) C47 0.031(3) 0.053(5) 0.032(3) 0.005(3) -0.001(3) 0.005(3) F1 0.056(3) 0.049(3) 0.064(3) -0.006(2) -0.006(2) 0.016(2) F2 0.039(2) 0.073(3) 0.047(2) 0.019(2) 0.0114(18) 0.020(2) F3 0.062(3) 0.071(3) 0.030(2) 0.019(2) 0.0078(19) 0.016(2) C44 0.037(4) 0.049(5) 0.031(3) 0.006(3) 0.006(3) -0.004(3) C48 0.051(4) 0.057(5) 0.036(4) 0.006(4) 0.008(3) -0.001(4) F4 0.096(4) 0.080(4) 0.037(2) 0.018(3) 0.021(2) -0.001(3) F5 0.114(5) 0.060(4) 0.102(4) -0.005(3) 0.054(4) -0.029(3) F6 0.063(3) 0.138(6) 0.058(3) 0.046(3) -0.002(2) -0.019(3) C49 0.035(4) 0.037(4) 0.036(4) -0.005(3) 0.008(3) -0.003(3) F7 0.100(7) 0.037(3) 0.045(4) 0.009(4) 0.029(4) 0.008(3) F8 0.084(5) 0.062(5) 0.027(3) -0.034(4) -0.014(3) 0.010(3) F9 0.042(4) 0.101(7) 0.052(4) 0.013(4) 0.014(3) 0.028(4) F7A 0.065(14) 0.096(19) 0.062(13) 0.009(13) 0.000(11) 0.026(13) F8A 0.12(2) 0.078(16) 0.076(16) -0.007(16) 0.035(16) 0.012(13) F9A 0.079(16) 0.082(17) 0.084(15) -0.016(14) -0.006(12) -0.012(13) 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C9 N1 C7 . . 114.1(5) ? C9 N1 C11 . . 122.7(5) ? C7 N1 C11 . . 122.1(5) ? C8 N3 C31 . . 121.8(5) ? C7 C1 C5 . . 123.1(6) ? C7 C1 C2 . . 129.5(6) ? C5 C1 C2 . . 107.4(6) ? C3 C2 C1 . . 104.2(6) ? C3 C2 H2A . . 110.9 ? C1 C2 H2A . . 110.9 ? C3 C2 H2B . . 110.9 ? C1 C2 H2B . . 110.9 ? H2A C2 H2B . . 108.9 ? C4 C3 C2 . . 104.2(6) ? C4 C3 H3A . . 110.9 ? C2 C3 H3A . . 110.9 ? C4 C3 H3B . . 110.9 ? C2 C3 H3B . . 110.9 ? H3A C3 H3B . . 108.9 ? C3 C4 C5 . . 104.0(6) ? C3 C4 H4A . . 111.0 ? C5 C4 H4A . . 111.0 ? C3 C4 H4B . . 111.0 ? C5 C4 H4B . . 111.0 ? H4A C4 H4B . . 109.0 ? C1 C5 C4 . . 105.4(6) ? C1 C5 H5A . . 110.7 ? C4 C5 H5A . . 110.7 ? C1 C5 H5B . . 110.7 ? C4 C5 H5B . . 110.7 ? H5A C5 H5B . . 108.8 ? C1 C7 N1 . . 124.9(6) ? C1 C7 C8 . . 127.7(6) ? N1 C7 C8 . . 107.4(5) ? N3 C8 C7 . . 117.9(6) ? N3 C8 B1 . . 133.9(6) ? C7 C8 B1 . . 108.2(5) ? N1 C9 N2 . . 117.3(6) ? N1 C9 B1 . . 112.1(5) ? N2 C9 B1 . . 130.2(6) ? C16 C11 C12 . . 123.5(6) ? C16 C11 N1 . . 118.3(6) ? C12 C11 N1 . . 118.2(6) ? C13 C12 C11 . . 117.4(7) ? C13 C12 C17 . . 121.0(7) ? C11 C12 C17 . . 121.4(7) ? C14 C13 C12 . . 121.2(8) ? C14 C13 H13 . . 119.4 ? C12 C13 H13 . . 119.4 ? C13 C14 C15 . . 121.2(8) ? C13 C14 H14 . . 119.4 ? C15 C14 H14 . . 119.4 ? C14 C15 C16 . . 121.1(8) ? C14 C15 H15 . . 119.5 ? C16 C15 H15 . . 119.5 ? C11 C16 C15 . . 115.6(7) ? C11 C16 C18 . . 123.4(7) ? C15 C16 C18 . . 121.0(8) ? C12 C17 H17A . . 109.5 ? C12 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C12 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C16 C18 H18A . . 109.5 ? C16 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C16 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? C9 N2 C21A . . 124.(3) ? C9 N2 C21 . . 125.7(14) ? C9 N2 H2 . . 121.(4) ? C21A N2 H2 . . 112.(5) ? C21 N2 H2 . . 106.(4) ? C22 C21 C26 . . 121.1(11) ? C22 C21 N2 . . 119.4(11) ? C26 C21 N2 . . 119.5(11) ? C21 C22 C23 . . 118.4(13) ? C21 C22 C27 . . 121.2(12) ? C23 C22 C27 . . 120.4(14) ? C24 C23 C22 . . 120.8(12) ? C24 C23 H23 . . 119.6 ? C22 C23 H23 . . 119.6 ? C25 C24 C23 . . 120.4(11) ? C25 C24 H24 . . 119.8 ? C23 C24 H24 . . 119.8 ? C24 C25 C26 . . 120.1(12) ? C24 C25 H25 . . 120.0 ? C26 C25 H25 . . 120.0 ? C25 C26 C21 . . 119.1(13) ? C25 C26 C28 . . 117.6(12) ? C21 C26 C28 . . 123.0(12) ? C22 C27 H27A . . 109.5 ? C22 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C22 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C26 C28 H28A . . 109.5 ? C26 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C26 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C22A C21A C26A . . 122.(2) ? C22A C21A N2 . . 118.2(19) ? C26A C21A N2 . . 117.8(19) ? C21A C22A C23A . . 119.(2) ? C21A C22A C27A . . 120.(2) ? C23A C22A C27A . . 120.(2) ? C24A C23A C22A . . 118.(2) ? C24A C23A H23A . . 121.0 ? C22A C23A H23A . . 121.0 ? C23A C24A C25A . . 121.(2) ? C23A C24A H24A . . 119.4 ? C25A C24A H24A . . 119.4 ? C26A C25A C24A . . 122.(2) ? C26A C25A H25A . . 118.9 ? C24A C25A H25A . . 118.9 ? C25A C26A C21A . . 116.(2) ? C25A C26A C28A . . 121.(2) ? C21A C26A C28A . . 123.(2) ? C22A C27A H27D . . 109.5 ? C22A C27A H27E . . 109.5 ? H27D C27A H27E . . 109.5 ? C22A C27A H27F . . 109.5 ? H27D C27A H27F . . 109.5 ? H27E C27A H27F . . 109.5 ? C26A C28A H28D . . 109.5 ? C26A C28A H28E . . 109.5 ? H28D C28A H28E . . 109.5 ? C26A C28A H28F . . 109.5 ? H28D C28A H28F . . 109.5 ? H28E C28A H28F . . 109.5 ? C36 C31 C32 . . 120.1(6) ? C36 C31 N3 . . 119.3(7) ? C32 C31 N3 . . 119.9(6) ? C33 C32 C31 . . 119.0(7) ? C33 C32 C37 . . 119.6(7) ? C31 C32 C37 . . 121.5(6) ? C32 C33 C34 . . 120.9(8) ? C32 C33 H33 . . 119.5 ? C34 C33 H33 . . 119.5 ? C35 C34 C33 . . 119.2(7) ? C35 C34 H34 . . 120.4 ? C33 C34 H34 . . 120.4 ? C34 C35 C36 . . 120.9(8) ? C34 C35 H35 . . 119.5 ? C36 C35 H35 . . 119.5 ? C31 C36 C35 . . 119.5(7) ? C31 C36 C38 . . 120.7(6) ? C35 C36 C38 . . 119.8(7) ? C32 C37 H37A . . 109.5 ? C32 C37 H37B . . 109.5 ? H37A C37 H37B . . 109.5 ? C32 C37 H37C . . 109.5 ? H37A C37 H37C . . 109.5 ? H37B C37 H37C . . 109.5 ? C36 C38 H38A . . 109.5 ? C36 C38 H38B . . 109.5 ? H38A C38 H38B . . 109.5 ? C36 C38 H38C . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? C9 B1 C8 . . 98.2(5) ? C9 B1 C41 . . 124.0(6) ? C8 B1 C41 . . 112.6(5) ? C9 B1 H1 . . 103.(3) ? C8 B1 H1 . . 105.(3) ? C41 B1 H1 . . 112.(3) ? C46 C41 C42 . . 113.7(6) ? C46 C41 B1 . . 124.3(6) ? C42 C41 B1 . . 120.8(6) ? C43 C42 C41 . . 122.7(6) ? C43 C42 C47 . . 115.8(6) ? C41 C42 C47 . . 121.5(6) ? C44 C43 C42 . . 121.0(6) ? C44 C43 H43 . . 119.5 ? C42 C43 H43 . . 119.5 ? C46 C45 C44 . . 119.3(7) ? C46 C45 H45 . . 120.4 ? C44 C45 H45 . . 120.4 ? C45 C46 C41 . . 123.5(6) ? C45 C46 C49 . . 114.2(6) ? C41 C46 C49 . . 122.4(6) ? F1 C47 F2 . . 106.6(6) ? F1 C47 F3 . . 106.3(6) ? F2 C47 F3 . . 104.6(5) ? F1 C47 C42 . . 114.6(5) ? F2 C47 C42 . . 113.2(6) ? F3 C47 C42 . . 110.8(6) ? C43 C44 C45 . . 119.3(7) ? C43 C44 C48 . . 122.0(7) ? C45 C44 C48 . . 118.7(7) ? F4 C48 F5 . . 105.2(7) ? F4 C48 F6 . . 106.9(6) ? F5 C48 F6 . . 105.6(8) ? F4 C48 C44 . . 112.8(7) ? F5 C48 C44 . . 113.4(7) ? F6 C48 C44 . . 112.3(6) ? F7 C49 F9 . . 105.6(7) ? F7 C49 F8 . . 106.9(7) ? F9 C49 F8 . . 103.5(6) ? F8A C49 F7A . . 108.(2) ? F8A C49 F9A . . 104.3(19) ? F7A C49 F9A . . 102.1(19) ? F8A C49 C46 . . 120.1(14) ? F7 C49 C46 . . 114.2(6) ? F9 C49 C46 . . 112.1(6) ? F8 C49 C46 . . 113.7(6) ? F7A C49 C46 . . 111.8(11) ? F9A C49 C46 . . 108.9(12) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C9 . 1.342(8) ? N1 C7 . 1.443(8) ? N1 C11 . 1.453(8) ? N3 C8 . 1.283(8) ? N3 C31 . 1.422(8) ? C1 C7 . 1.352(9) ? C1 C5 . 1.506(9) ? C1 C2 . 1.527(9) ? C2 C3 . 1.520(10) ? C2 H2A . 0.99 ? C2 H2B . 0.99 ? C3 C4 . 1.492(11) ? C3 H3A . 0.99 ? C3 H3B . 0.99 ? C4 C5 . 1.527(9) ? C4 H4A . 0.99 ? C4 H4B . 0.99 ? C5 H5A . 0.99 ? C5 H5B . 0.99 ? C7 C8 . 1.503(9) ? C8 B1 . 1.633(9) ? C9 N2 . 1.344(8) ? C9 B1 . 1.607(9) ? C11 C16 . 1.395(10) ? C11 C12 . 1.398(10) ? C12 C13 . 1.384(11) ? C12 C17 . 1.498(11) ? C13 C14 . 1.357(13) ? C13 H13 . 0.95 ? C14 C15 . 1.369(14) ? C14 H14 . 0.95 ? C15 C16 . 1.422(11) ? C15 H15 . 0.95 ? C16 C18 . 1.484(12) ? C17 H17A . 0.98 ? C17 H17B . 0.98 ? C17 H17C . 0.98 ? C18 H18A . 0.98 ? C18 H18B . 0.98 ? C18 H18C . 0.98 ? N2 C21A . 1.460(19) ? N2 C21 . 1.467(12) ? N2 H2 . 0.97(8) ? C21 C22 . 1.388(15) ? C21 C26 . 1.401(15) ? C22 C23 . 1.390(13) ? C22 C27 . 1.499(18) ? C23 C24 . 1.383(14) ? C23 H23 . 0.95 ? C24 C25 . 1.379(15) ? C24 H24 . 0.95 ? C25 C26 . 1.386(14) ? C25 H25 . 0.95 ? C26 C28 . 1.525(18) ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C21A C22A . 1.388(19) ? C21A C26A . 1.40(2) ? C22A C23A . 1.389(18) ? C22A C27A . 1.50(2) ? C23A C24A . 1.370(19) ? C23A H23A . 0.95 ? C24A C25A . 1.372(19) ? C24A H24A . 0.95 ? C25A C26A . 1.372(18) ? C25A H25A . 0.95 ? C26A C28A . 1.50(2) ? C27A H27D . 0.98 ? C27A H27E . 0.98 ? C27A H27F . 0.98 ? C28A H28D . 0.98 ? C28A H28E . 0.98 ? C28A H28F . 0.98 ? C31 C36 . 1.381(11) ? C31 C32 . 1.401(10) ? C32 C33 . 1.386(10) ? C32 C37 . 1.513(11) ? C33 C34 . 1.388(12) ? C33 H33 . 0.95 ? C34 C35 . 1.374(12) ? C34 H34 . 0.95 ? C35 C36 . 1.393(10) ? C35 H35 . 0.95 ? C36 C38 . 1.521(11) ? C37 H37A . 0.98 ? C37 H37B . 0.98 ? C37 H37C . 0.98 ? C38 H38A . 0.98 ? C38 H38B . 0.98 ? C38 H38C . 0.98 ? B1 C41 . 1.636(10) ? B1 H1 . 1.15(7) ? C41 C46 . 1.415(10) ? C41 C42 . 1.433(9) ? C42 C43 . 1.373(10) ? C42 C47 . 1.505(10) ? C43 C44 . 1.369(11) ? C43 H43 . 0.95 ? C45 C46 . 1.388(10) ? C45 C44 . 1.399(10) ? C45 H45 . 0.95 ? C46 C49 . 1.515(9) ? C47 F1 . 1.331(9) ? C47 F2 . 1.343(8) ? C47 F3 . 1.347(8) ? C44 C48 . 1.493(10) ? C48 F4 . 1.315(9) ? C48 F5 . 1.318(10) ? C48 F6 . 1.320(9) ? C49 F8A . 1.295(17) ? C49 F7 . 1.309(9) ? C49 F9 . 1.332(8) ? C49 F8 . 1.336(8) ? C49 F7A . 1.342(16) ? C49 F9A . 1.357(17) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C7 C1 C2 C3 . . . . 164.5(8) ? C5 C1 C2 C3 . . . . -15.1(9) ? C1 C2 C3 C4 . . . . 33.5(9) ? C2 C3 C4 C5 . . . . -39.1(9) ? C7 C1 C5 C4 . . . . 171.9(7) ? C2 C1 C5 C4 . . . . -8.6(9) ? C3 C4 C5 C1 . . . . 29.5(9) ? C5 C1 C7 N1 . . . . -176.2(7) ? C2 C1 C7 N1 . . . . 4.3(13) ? C5 C1 C7 C8 . . . . 4.4(12) ? C2 C1 C7 C8 . . . . -175.1(8) ? C9 N1 C7 C1 . . . . -179.0(7) ? C11 N1 C7 C1 . . . . 12.9(11) ? C9 N1 C7 C8 . . . . 0.5(8) ? C11 N1 C7 C8 . . . . -167.5(6) ? C31 N3 C8 C7 . . . . -176.1(6) ? C31 N3 C8 B1 . . . . 2.6(13) ? C1 C7 C8 N3 . . . . 0.7(11) ? N1 C7 C8 N3 . . . . -178.8(6) ? C1 C7 C8 B1 . . . . -178.4(7) ? N1 C7 C8 B1 . . . . 2.1(8) ? C7 N1 C9 N2 . . . . -176.5(6) ? C11 N1 C9 N2 . . . . -8.5(10) ? C7 N1 C9 B1 . . . . -3.1(8) ? C11 N1 C9 B1 . . . . 164.9(6) ? C9 N1 C11 C16 . . . . 89.6(8) ? C7 N1 C11 C16 . . . . -103.4(8) ? C9 N1 C11 C12 . . . . -90.8(8) ? C7 N1 C11 C12 . . . . 76.3(8) ? C16 C11 C12 C13 . . . . 1.7(11) ? N1 C11 C12 C13 . . . . -178.0(6) ? C16 C11 C12 C17 . . . . 176.7(7) ? N1 C11 C12 C17 . . . . -2.9(10) ? C11 C12 C13 C14 . . . . -0.3(12) ? C17 C12 C13 C14 . . . . -175.4(8) ? C12 C13 C14 C15 . . . . 0.0(13) ? C13 C14 C15 C16 . . . . -1.0(13) ? C12 C11 C16 C15 . . . . -2.6(11) ? N1 C11 C16 C15 . . . . 177.1(6) ? C12 C11 C16 C18 . . . . -179.6(8) ? N1 C11 C16 C18 . . . . 0.1(11) ? C14 C15 C16 C11 . . . . 2.2(12) ? C14 C15 C16 C18 . . . . 179.3(8) ? N1 C9 N2 C21A . . . . 175.7(14) ? B1 C9 N2 C21A . . . . 3.6(18) ? N1 C9 N2 C21 . . . . 163.7(10) ? B1 C9 N2 C21 . . . . -8.3(14) ? C9 N2 C21 C22 . . . . -79.(3) ? C9 N2 C21 C26 . . . . 101.(2) ? C26 C21 C22 C23 . . . . 2.(4) ? N2 C21 C22 C23 . . . . -178.(2) ? C26 C21 C22 C27 . . . . -180.(2) ? N2 C21 C22 C27 . . . . 0.(4) ? C21 C22 C23 C24 . . . . -2.(3) ? C27 C22 C23 C24 . . . . 179.6(18) ? C22 C23 C24 C25 . . . . 3.(2) ? C23 C24 C25 C26 . . . . -3.(2) ? C24 C25 C26 C21 . . . . 3.(3) ? C24 C25 C26 C28 . . . . 177.0(16) ? C22 C21 C26 C25 . . . . -2.(4) ? N2 C21 C26 C25 . . . . 178.(2) ? C22 C21 C26 C28 . . . . -176.(2) ? N2 C21 C26 C28 . . . . 4.(4) ? C9 N2 C21A C22A . . . . -90.(6) ? C9 N2 C21A C26A . . . . 107.(5) ? C26A C21A C22A C23A . . . . -12.(9) ? N2 C21A C22A C23A . . . . -175.(4) ? C26A C21A C22A C27A . . . . 172.(5) ? N2 C21A C22A C27A . . . . 9.(9) ? C21A C22A C23A C24A . . . . 0.(7) ? C27A C22A C23A C24A . . . . 175.(4) ? C22A C23A C24A C25A . . . . 9.(5) ? C23A C24A C25A C26A . . . . -5.(6) ? C24A C25A C26A C21A . . . . -7.(6) ? C24A C25A C26A C28A . . . . 175.(4) ? C22A C21A C26A C25A . . . . 15.(9) ? N2 C21A C26A C25A . . . . 178.(4) ? C22A C21A C26A C28A . . . . -166.(5) ? N2 C21A C26A C28A . . . . -3.(8) ? C8 N3 C31 C36 . . . . 82.5(9) ? C8 N3 C31 C32 . . . . -107.6(8) ? C36 C31 C32 C33 . . . . -7.7(10) ? N3 C31 C32 C33 . . . . -177.5(6) ? C36 C31 C32 C37 . . . . 169.9(6) ? N3 C31 C32 C37 . . . . 0.2(10) ? C31 C32 C33 C34 . . . . 3.7(10) ? C37 C32 C33 C34 . . . . -173.9(7) ? C32 C33 C34 C35 . . . . 1.7(11) ? C33 C34 C35 C36 . . . . -3.2(11) ? C32 C31 C36 C35 . . . . 6.3(10) ? N3 C31 C36 C35 . . . . 176.1(6) ? C32 C31 C36 C38 . . . . -172.0(6) ? N3 C31 C36 C38 . . . . -2.2(10) ? C34 C35 C36 C31 . . . . -0.8(11) ? C34 C35 C36 C38 . . . . 177.5(7) ? N1 C9 B1 C8 . . . . 3.9(7) ? N2 C9 B1 C8 . . . . 176.3(7) ? N1 C9 B1 C41 . . . . 128.3(7) ? N2 C9 B1 C41 . . . . -59.3(11) ? N3 C8 B1 C9 . . . . 177.7(8) ? C7 C8 B1 C9 . . . . -3.4(7) ? N3 C8 B1 C41 . . . . 45.5(11) ? C7 C8 B1 C41 . . . . -135.6(6) ? C9 B1 C41 C46 . . . . -62.5(9) ? C8 B1 C41 C46 . . . . 55.3(8) ? C9 B1 C41 C42 . . . . 130.9(7) ? C8 B1 C41 C42 . . . . -111.3(7) ? C46 C41 C42 C43 . . . . -7.8(9) ? B1 C41 C42 C43 . . . . 160.1(6) ? C46 C41 C42 C47 . . . . 169.7(6) ? B1 C41 C42 C47 . . . . -22.4(9) ? C41 C42 C43 C44 . . . . 3.6(10) ? C47 C42 C43 C44 . . . . -174.0(6) ? C44 C45 C46 C41 . . . . 1.6(10) ? C44 C45 C46 C49 . . . . -179.4(6) ? C42 C41 C46 C45 . . . . 5.2(9) ? B1 C41 C46 C45 . . . . -162.3(6) ? C42 C41 C46 C49 . . . . -173.7(6) ? B1 C41 C46 C49 . . . . 18.9(10) ? C43 C42 C47 F1 . . . . -103.2(7) ? C41 C42 C47 F1 . . . . 79.1(8) ? C43 C42 C47 F2 . . . . 134.2(6) ? C41 C42 C47 F2 . . . . -43.5(9) ? C43 C42 C47 F3 . . . . 17.0(8) ? C41 C42 C47 F3 . . . . -160.7(6) ? C42 C43 C44 C45 . . . . 3.8(10) ? C42 C43 C44 C48 . . . . -175.4(7) ? C46 C45 C44 C43 . . . . -6.4(10) ? C46 C45 C44 C48 . . . . 172.9(7) ? C43 C44 C48 F4 . . . . -10.1(11) ? C45 C44 C48 F4 . . . . 170.7(7) ? C43 C44 C48 F5 . . . . -129.6(8) ? C45 C44 C48 F5 . . . . 51.2(10) ? C43 C44 C48 F6 . . . . 110.8(9) ? C45 C44 C48 F6 . . . . -68.4(10) ? C45 C46 C49 F8A . . . . 178.(2) ? C41 C46 C49 F8A . . . . -3.(2) ? C45 C46 C49 F7 . . . . -0.8(9) ? C41 C46 C49 F7 . . . . 178.1(7) ? C45 C46 C49 F9 . . . . -120.9(7) ? C41 C46 C49 F9 . . . . 58.1(9) ? C45 C46 C49 F8 . . . . 122.2(7) ? C41 C46 C49 F8 . . . . -58.8(9) ? C45 C46 C49 F7A . . . . 50.4(18) ? C41 C46 C49 F7A . . . . -130.7(17) ? C45 C46 C49 F9A . . . . -61.7(16) ? C41 C46 C49 F9A . . . . 117.2(16) ?