#------------------------------------------------------------------------------ #$Date: 2021-07-15 06:52:57 +0300 (Thu, 15 Jul 2021) $ #$Revision: 267545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/81/7158170.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_7158170 loop_ _publ_author_name 'Wang, Baomin' 'Nawaz, Shah' 'Wei, Shiqiang' 'Huang, Yue' 'Wang, Wenyao' 'Qu, Jingping' _publ_section_title ; Diastereoselective synthesis of indolenine-based spiro[pyrazolone-4,2’-pyrrolidine] scaffolds via 1,3-dipolar cycloaddition of 4-aminopyrazolones, aldehydes, and indolenines ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/D1OB01135A _journal_year 2021 _chemical_formula_moiety 'C40 H33 Br N4 O' _chemical_formula_sum 'C40 H33 Br N4 O' _chemical_formula_weight 665.61 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-06-11 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2021-06-12 deposited with the CCDC. 2021-07-13 downloaded from the CCDC. ; _cell_angle_alpha 75.801(2) _cell_angle_beta 69.663(2) _cell_angle_gamma 66.4250(10) _cell_formula_units_Z 2 _cell_length_a 12.2987(7) _cell_length_b 12.4224(7) _cell_length_c 13.2018(8) _cell_measurement_reflns_used 9966 _cell_measurement_temperature 296.0 _cell_measurement_theta_max 25.462 _cell_measurement_theta_min 2.168 _cell_volume 1720.08(17) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296.0 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 32619 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.550 _diffrn_reflns_theta_min 1.802 _diffrn_source_current 50.0 _diffrn_source_power 2.5 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5766 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1135 before and 0.0519 after correction. The Ratio of minimum to maximum transmission is 0.7733. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'light colourless' _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.285 _exptl_crystal_description block _exptl_crystal_F_000 688 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.755 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 421 _refine_ls_number_reflns 7890 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0494 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0806P)^2^+0.5388P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1373 _refine_ls_wR_factor_ref 0.1582 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5061 _reflns_number_total 7890 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ob01135a2.cif _cod_data_source_block 2 _cod_original_cell_volume 1720.08(18) _cod_database_code 7158170 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.952 _shelx_estimated_absorpt_t_min 0.908 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C16(H16), C23(H23), C24(H24) 2.b Aromatic/amide H refined with riding coordinates: C40(H40), C38(H38), C37(H37), C17(H17), C15(H15), C19(H19), C11(H11), C20(H20), C26(H26), C14(H14), C3(H3A), C30(H30), C22(H22), C13(H13), C21(H21), C12(H12), C27(H27), C2(H2), C28(H28), C5(H5), C1(H1), C29(H29), C6(H6) 2.c Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C33(H33A,H33B,H33C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 2_a.res in P-1 2.res created by SHELXL-2018/3 at 14:17:07 on 11-Jun-2021 REM Old TITL 2 in P-1 REM SHELXT solution in P-1: R1 0.218, Rweak 0.032, Alpha 0.060 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C40 N3 O3 Br CELL 0.71073 12.2987 12.4224 13.2018 75.801 69.663 66.425 ZERR 2 0.0007 0.0007 0.0008 0.002 0.002 0.001 LATT 1 SFAC C H Br N O UNIT 80 66 2 8 2 L.S. 20 PLAN 10 SIZE 0.04 0.06 0.08 TEMP 22.85 CONF list 4 fmap 2 53 MORE -1 ACTA ABIN BOND $H REM REM REM WGHT 0.080600 0.538800 FVAR 0.92989 BR1 3 -0.099047 -0.115284 0.945404 11.00000 0.07644 0.08620 = 0.08109 0.00489 -0.01018 -0.04938 O1 5 0.560470 0.283254 0.389191 11.00000 0.04575 0.04651 = 0.08425 -0.01439 -0.00455 -0.00211 N4 4 0.116084 0.264946 0.701247 11.00000 0.03881 0.04112 = 0.05247 -0.01041 -0.00525 -0.00858 N3 4 0.409470 0.402639 0.584747 11.00000 0.04599 0.04067 = 0.06694 -0.00290 -0.02481 -0.01344 N2 4 0.370283 0.572751 0.337236 11.00000 0.04686 0.03966 = 0.06120 -0.00711 -0.00899 -0.01423 N1 4 0.467033 0.467125 0.304180 11.00000 0.04615 0.04349 = 0.05630 -0.01234 -0.00246 -0.01514 C31 1 0.228557 0.201184 0.658276 11.00000 0.03814 0.03823 = 0.04388 -0.00811 -0.01000 -0.00958 C16 1 0.275044 0.365439 0.513676 11.00000 0.03411 0.03478 = 0.04948 -0.00717 -0.00960 -0.00889 AFIX 13 H16 2 0.196984 0.417491 0.556058 11.00000 -1.20000 AFIX 0 C35 1 0.128663 0.068258 0.750672 11.00000 0.04166 0.04307 = 0.05037 -0.00861 -0.01061 -0.01246 C8 1 0.372194 0.427449 0.486276 11.00000 0.03749 0.03613 = 0.05643 -0.00732 -0.01236 -0.01034 C36 1 0.051718 0.186053 0.758889 11.00000 0.04038 0.04655 = 0.04541 -0.01011 -0.00592 -0.01169 C23 1 0.322485 0.257390 0.593335 11.00000 0.03528 0.03574 = 0.04761 -0.00855 -0.00913 -0.00740 AFIX 13 H23 2 0.396372 0.198769 0.553363 11.00000 -1.20000 AFIX 0 C7 1 0.479773 0.380093 0.388711 11.00000 0.03947 0.04321 = 0.06302 -0.01007 -0.00881 -0.01531 C40 1 0.084619 -0.022314 0.804858 11.00000 0.05038 0.04843 = 0.06122 -0.00641 -0.01285 -0.01832 AFIX 43 H40 2 0.135310 -0.101111 0.800401 11.00000 -1.20000 AFIX 0 C9 1 0.320149 0.554184 0.439223 11.00000 0.03751 0.03609 = 0.05443 -0.00874 -0.01264 -0.01197 C10 1 0.217513 0.649219 0.497390 11.00000 0.03871 0.03491 = 0.06452 -0.00846 -0.01167 -0.01142 C18 1 0.249041 0.346602 0.417786 11.00000 0.04278 0.04284 = 0.04858 -0.00261 -0.01105 -0.01962 C32 1 0.254200 0.067771 0.679881 11.00000 0.03818 0.03686 = 0.05803 -0.00808 -0.00686 -0.01139 C38 1 -0.115159 0.124188 0.873019 11.00000 0.04486 0.08158 = 0.05733 -0.01756 0.00205 -0.02628 AFIX 43 H38 2 -0.197300 0.141411 0.914288 11.00000 -1.20000 AFIX 0 C24 1 0.359242 0.314418 0.662652 11.00000 0.04392 0.04051 = 0.05387 -0.00836 -0.01490 -0.01010 AFIX 13 H24 2 0.283434 0.357317 0.714554 11.00000 -1.20000 AFIX 0 C37 1 -0.070868 0.215039 0.818631 11.00000 0.04595 0.05874 = 0.06201 -0.01590 -0.00115 -0.01200 AFIX 43 H37 2 -0.122351 0.293699 0.822196 11.00000 -1.20000 AFIX 0 C39 1 -0.037961 0.008216 0.866256 11.00000 0.05386 0.06308 = 0.05363 -0.00516 -0.00951 -0.02891 C34 1 0.288531 0.017590 0.573539 11.00000 0.06181 0.04999 = 0.07253 -0.02297 0.00435 -0.02112 AFIX 137 H34A 2 0.226402 0.062309 0.536309 11.00000 -1.50000 H34B 2 0.293778 -0.063715 0.589470 11.00000 -1.50000 H34C 2 0.366935 0.022716 0.528168 11.00000 -1.50000 AFIX 0 C17 1 0.147572 0.428502 0.384276 11.00000 0.04484 0.06110 = 0.06089 -0.00160 -0.01555 -0.02074 AFIX 43 H17 2 0.097113 0.493508 0.421844 11.00000 -1.20000 AFIX 0 C25 1 0.446439 0.230291 0.725846 11.00000 0.06683 0.04358 = 0.07315 0.00383 -0.03820 -0.02188 C15 1 0.191946 0.647164 0.608255 11.00000 0.05735 0.04568 = 0.06836 -0.01488 -0.01010 -0.01036 AFIX 43 H15 2 0.239082 0.584081 0.647506 11.00000 -1.20000 AFIX 0 C33 1 0.353896 -0.000626 0.739266 11.00000 0.04976 0.04250 = 0.09991 0.00435 -0.02569 -0.01325 AFIX 137 H33A 2 0.430982 0.008275 0.694668 11.00000 -1.50000 H33B 2 0.363134 -0.082945 0.753479 11.00000 -1.50000 H33C 2 0.330033 0.029943 0.806856 11.00000 -1.50000 AFIX 0 C19 1 0.323555 0.252144 0.358642 11.00000 0.06844 0.04805 = 0.05943 -0.00770 -0.01965 -0.01872 AFIX 43 H19 2 0.392629 0.197083 0.378945 11.00000 -1.20000 AFIX 0 C4 1 0.543367 0.469752 0.195903 11.00000 0.06383 0.05991 = 0.06170 -0.01722 0.00168 -0.03258 C11 1 0.145704 0.743673 0.441039 11.00000 0.06281 0.04950 = 0.08467 -0.00556 -0.02583 -0.00656 AFIX 43 H11 2 0.161656 0.746702 0.366371 11.00000 -1.20000 AFIX 0 C20 1 0.297380 0.238110 0.270273 11.00000 0.10215 0.06801 = 0.05838 -0.01331 -0.01675 -0.04053 AFIX 43 H20 2 0.348240 0.174327 0.231203 11.00000 -1.20000 AFIX 0 C26 1 0.566735 0.167009 0.674314 11.00000 0.05638 0.05104 = 0.11857 0.00846 -0.04053 -0.01612 AFIX 43 H26 2 0.595366 0.176763 0.598732 11.00000 -1.20000 AFIX 0 C14 1 0.095704 0.739447 0.661162 11.00000 0.07472 0.06009 = 0.08374 -0.02929 0.00140 -0.01657 AFIX 43 H14 2 0.079193 0.738093 0.735672 11.00000 -1.20000 AFIX 0 C3 1 0.515803 0.568777 0.123125 11.00000 0.09395 0.06512 = 0.06693 -0.01197 0.00103 -0.03509 AFIX 43 H3A 2 0.446739 0.634744 0.144934 11.00000 -1.20000 AFIX 0 C30 1 0.406581 0.213370 0.838213 11.00000 0.11508 0.06599 = 0.07522 0.00451 -0.04909 -0.03508 AFIX 43 H30 2 0.325979 0.255932 0.874249 11.00000 -1.20000 AFIX 0 C22 1 0.120796 0.414731 0.296398 11.00000 0.06947 0.09606 = 0.06997 0.00667 -0.03560 -0.03369 AFIX 43 H22 2 0.052402 0.469993 0.275173 11.00000 -1.20000 AFIX 0 C13 1 0.026446 0.830530 0.605289 11.00000 0.05789 0.05287 = 0.12271 -0.03232 0.00113 -0.00548 AFIX 43 H13 2 -0.037864 0.891649 0.641445 11.00000 -1.20000 AFIX 0 C21 1 0.194372 0.320244 0.240493 11.00000 0.10314 0.10332 = 0.06505 -0.00166 -0.03534 -0.05879 AFIX 43 H21 2 0.175255 0.310773 0.181719 11.00000 -1.20000 AFIX 0 C12 1 0.049787 0.833937 0.496124 11.00000 0.06572 0.05000 = 0.12839 -0.01100 -0.03339 0.00564 AFIX 43 H12 2 0.001105 0.897191 0.458252 11.00000 -1.20000 AFIX 0 C27 1 0.645097 0.088728 0.735298 11.00000 0.07969 0.06028 = 0.20673 0.02802 -0.08447 -0.02521 AFIX 43 H27 2 0.726731 0.047576 0.700427 11.00000 -1.20000 AFIX 0 C2 1 0.590317 0.571144 0.017166 11.00000 0.13898 0.08718 = 0.06790 -0.00851 0.00502 -0.05775 AFIX 43 H2 2 0.571035 0.638748 -0.032131 11.00000 -1.20000 AFIX 0 C28 1 0.603358 0.072001 0.845123 11.00000 0.16892 0.07534 = 0.20471 0.05843 -0.15130 -0.05929 AFIX 43 H28 2 0.655652 0.017790 0.885363 11.00000 -1.20000 AFIX 0 C5 1 0.646661 0.372098 0.164034 11.00000 0.08616 0.08030 = 0.07751 -0.02028 0.01563 -0.01206 AFIX 43 H5 2 0.666126 0.304339 0.213127 11.00000 -1.20000 AFIX 0 C1 1 0.691295 0.475659 -0.015434 11.00000 0.13718 0.10558 = 0.07850 -0.03491 0.03851 -0.06083 AFIX 43 H1 2 0.740419 0.477192 -0.087169 11.00000 -1.20000 AFIX 0 C29 1 0.484563 0.134560 0.897062 11.00000 0.20933 0.08505 = 0.11789 0.03773 -0.11162 -0.06937 AFIX 43 H29 2 0.456535 0.123601 0.972648 11.00000 -1.20000 AFIX 0 C6 1 0.720723 0.376912 0.057649 11.00000 0.11410 0.10681 = 0.09064 -0.03028 0.02958 -0.02214 AFIX 43 H6 2 0.791315 0.312249 0.035608 11.00000 -1.20000 AFIX 0 H3 2 0.485236 0.381323 0.569235 11.00000 0.05298 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.1582, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0494 for 5061 Fo > 4sig(Fo) and 0.0850 for all 7890 data REM 421 parameters refined using 0 restraints END WGHT 0.0807 0.5372 REM Highest difference peak 0.755, deepest hole -0.627, 1-sigma level 0.050 Q1 1 -0.1200 -0.0970 0.8850 11.00000 0.05 0.76 Q2 1 -0.1392 -0.0575 0.9841 11.00000 0.05 0.65 Q3 1 0.1534 0.2939 0.9543 11.00000 0.05 0.24 Q4 1 -0.0637 -0.1335 0.9459 11.00000 0.05 0.22 Q5 1 0.2990 0.3012 0.5533 11.00000 0.05 0.21 Q6 1 0.0959 0.1166 0.7730 11.00000 0.05 0.20 Q7 1 0.0851 0.1222 0.7346 11.00000 0.05 0.20 Q8 1 0.2008 0.0592 0.7209 11.00000 0.05 0.20 Q9 1 0.7501 0.0320 0.6329 11.00000 0.05 0.20 Q10 1 0.5630 0.1210 0.8678 11.00000 0.05 0.19 ; _shelx_res_checksum 85491 _shelx_fab_file ; -14 -9 1 -0.3594 0.0261 -14 -8 1 0.1308 -0.0020 -14 -7 1 -0.0129 -0.0056 -14 -7 2 -0.1135 -0.0448 -14 -6 1 -0.0774 -0.0075 -14 -6 2 0.0417 0.0256 -14 -5 1 0.2720 0.0339 -14 -5 2 0.0631 0.0119 -14 -4 1 -0.4402 -0.0511 -14 -4 2 -0.1420 -0.0351 -14 -3 1 0.4049 0.0419 -14 -3 2 0.1405 0.0293 -14 -2 1 -0.2752 -0.0213 -14 -1 1 0.2644 0.0174 -13 -11 1 -0.2623 0.0668 -13 -10 1 0.6211 -0.0709 -13 -10 2 0.5285 0.0078 -13 -9 1 -0.6569 0.0502 -13 -9 2 -0.5977 -0.0227 -13 -8 1 0.3990 -0.0198 -13 -8 2 0.3994 0.0232 -13 -8 3 0.3066 0.0396 -13 -7 1 -0.1252 0.0001 -13 -7 2 -0.1328 -0.0262 -13 -7 3 -0.1419 -0.0326 -13 -6 1 -0.0892 0.0012 -13 -6 2 -0.0925 0.0246 -13 -6 3 -0.0224 0.0346 -13 -6 4 -0.0774 0.0118 -13 -5 1 0.3779 0.0106 -13 -5 2 0.2927 -0.0046 -13 -5 3 0.1042 -0.0164 -13 -5 4 0.0623 -0.0022 -13 -4 1 -0.6752 -0.0224 -13 -4 2 -0.4207 -0.0196 -13 -4 3 -0.0791 -0.0081 -13 -4 4 0.0667 -0.0110 -13 -3 1 0.6948 0.0208 -13 -3 2 0.3672 0.0237 -13 -3 3 -0.0206 0.0138 -13 -3 4 -0.1899 0.0098 -13 -2 1 -0.4020 -0.0081 -13 -2 2 -0.1604 -0.0130 -13 -2 3 0.1364 -0.0103 -13 -2 4 0.2423 -0.0102 -13 -1 1 0.1399 0.0040 -13 -1 2 -0.0214 0.0119 -13 -1 3 -0.2162 0.0169 -13 0 1 -0.1380 -0.0144 -13 0 2 0.0702 -0.0204 -13 0 3 0.2153 -0.0240 -13 1 1 0.2161 0.0176 -13 1 2 -0.0404 0.0157 -13 2 1 -0.1461 -0.0010 -12 -12 1 0.0761 0.0064 -12 -11 1 -0.2350 0.0296 -12 -11 2 -0.3037 0.0352 -12 -10 1 0.5021 -0.0403 -12 -10 2 0.5902 -0.0274 -12 -10 3 0.2295 0.0128 -12 -9 1 -0.6689 0.0271 -12 -9 2 -0.7319 -0.0032 -12 -9 3 -0.3925 -0.0504 -12 -9 4 -0.0065 -0.0545 -12 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5 2.2327 -0.0056 2 -2 6 -2.1634 -0.0061 2 -2 7 -3.7312 0.0008 2 -2 8 -3.3847 0.0031 2 -2 9 -1.9828 0.0037 2 -2 10 -0.4726 0.0087 2 -2 11 0.4301 0.0115 2 -2 12 0.6755 0.0054 2 -2 13 0.4570 -0.0032 2 -2 14 -0.0147 -0.0062 2 -2 15 -0.3279 -0.0056 2 -1 0 -15.0620 0.0138 2 -1 1 -23.9966 0.0323 2 -1 2 -25.9329 0.0157 2 -1 3 -20.2567 -0.0177 2 -1 4 -9.6476 -0.0343 2 -1 5 0.3469 -0.0293 2 -1 6 5.6176 -0.0205 2 -1 7 6.1950 -0.0157 2 -1 8 4.2611 -0.0101 2 -1 9 1.6808 -0.0035 2 -1 10 -0.3669 -0.0002 2 -1 11 -1.3274 0.0012 2 -1 12 -1.3112 0.0052 2 -1 13 -0.7250 0.0087 2 -1 14 -0.0510 0.0048 2 -1 15 0.2603 -0.0048 2 -1 16 0.1843 -0.0127 2 0 0 23.7887 -0.0348 2 0 2 28.4131 -0.0312 2 0 3 19.5273 -0.0053 2 0 4 6.5254 0.0097 2 0 5 -4.4508 0.0101 2 0 6 -9.0327 0.0065 2 0 7 -7.8461 0.0046 2 0 8 -4.2089 0.0012 2 0 9 -0.7446 -0.0042 2 0 10 1.4096 -0.0060 2 0 11 2.0976 -0.0032 2 0 12 1.6922 -0.0014 2 0 13 0.7619 -0.0006 2 0 14 -0.0570 0.0049 2 0 15 -0.3329 0.0140 2 0 16 -0.2034 0.0167 2 1 0 -26.4018 0.0074 2 1 1 -28.1747 0.0019 2 1 2 -23.2564 0.0081 2 1 4 -0.3880 0.0304 2 1 5 8.8429 0.0279 2 1 6 11.1596 0.0184 2 1 7 7.9168 0.0084 2 1 8 3.0363 0.0040 2 1 9 -0.6573 0.0044 2 1 10 -2.3596 0.0012 2 1 11 -2.4256 -0.0059 2 1 12 -1.5258 -0.0076 2 1 13 -0.3353 -0.0021 2 1 14 0.4904 0.0007 2 1 15 0.6300 -0.0031 2 1 16 0.3656 -0.0058 2 2 0 22.5408 0.0432 2 2 1 20.1729 0.0587 2 2 2 13.2020 0.0340 2 2 3 3.5646 -0.0058 2 2 4 -6.0870 -0.0250 2 2 5 -11.7230 -0.0201 2 2 6 -11.1273 -0.0077 2 2 7 -6.2339 0.0010 2 2 8 -0.9065 0.0018 2 2 9 2.3490 -0.0017 2 2 10 3.1913 -0.0001 2 2 11 2.4393 0.0069 2 2 12 1.0334 0.0072 2 2 13 -0.2922 -0.0020 2 2 14 -0.9842 -0.0091 2 2 15 -0.9288 -0.0062 2 2 16 -0.5444 0.0013 2 3 1 -9.8352 -0.0554 2 3 2 -2.8428 -0.0360 2 3 3 4.4055 -0.0123 2 3 4 10.0660 -0.0092 2 3 5 11.7960 -0.0157 2 3 6 8.7817 -0.0159 2 3 7 3.1786 -0.0112 2 3 8 -1.7170 -0.0043 2 3 9 -4.0109 0.0037 2 3 10 -3.8116 0.0055 2 3 11 -2.2677 -0.0003 2 3 12 -0.4925 -0.0042 2 3 13 0.8001 -0.0012 2 3 14 1.2511 0.0026 2 3 15 0.9963 0.0016 2 3 16 0.5623 -0.0027 2 4 0 5.6278 -0.0113 2 4 1 0.7786 -0.0066 2 4 2 -4.4705 -0.0062 2 4 3 -8.4989 0.0011 2 4 4 -10.3208 0.0159 2 4 5 -9.0209 0.0185 2 4 6 -4.7981 0.0071 2 4 7 0.3481 -0.0002 2 4 8 3.9676 -0.0004 2 4 9 4.9137 -0.0021 2 4 10 3.7123 -0.0039 2 4 11 1.6730 -0.0008 2 4 12 -0.1300 0.0044 2 4 13 -1.1597 0.0070 2 4 14 -1.2917 0.0053 2 4 15 -0.8451 -0.0000 2 4 16 -0.3898 -0.0047 2 5 0 1.3326 0.0433 2 5 1 4.8589 0.0361 2 5 2 7.5473 0.0267 2 5 3 8.4675 0.0138 2 5 4 7.4361 0.0031 2 5 5 4.5410 0.0075 2 5 6 0.4896 0.0176 2 5 7 -3.1642 0.0140 2 5 8 -4.9193 0.0010 2 5 9 -4.4284 -0.0055 2 5 10 -2.5856 -0.0039 2 5 11 -0.6215 -0.0013 2 5 12 0.7478 -0.0012 2 5 13 1.3417 -0.0028 2 5 14 1.2049 -0.0009 2 5 15 0.6476 0.0075 2 5 16 0.1800 0.0142 2 6 0 -4.7233 -0.0090 2 6 1 -6.4672 0.0025 2 6 2 -6.8037 0.0032 2 6 3 -5.5184 -0.0019 2 6 4 -3.0671 -0.0058 2 6 5 -0.0606 -0.0108 2 6 6 2.7608 -0.0128 2 6 7 4.4417 -0.0061 2 6 8 4.3559 0.0027 2 6 9 2.8540 0.0056 2 6 10 1.0296 0.0037 2 6 11 -0.2556 -0.0005 2 6 12 -0.9075 -0.0039 2 6 13 -1.1477 -0.0028 2 6 14 -1.0021 -0.0019 2 6 15 -0.5310 -0.0070 2 6 16 -0.0919 -0.0108 2 7 0 4.7717 -0.0282 2 7 1 4.9725 -0.0361 2 7 2 3.7939 -0.0286 2 7 3 1.5782 -0.0134 2 7 4 -0.8848 -0.0073 2 7 5 -2.9451 -0.0107 2 7 6 -4.1706 -0.0137 2 7 7 -4.1662 -0.0096 2 7 8 -2.9120 -0.0005 2 7 9 -1.1635 0.0045 2 7 10 0.0497 0.0026 2 7 11 0.4103 0.0014 2 7 12 0.4431 0.0026 2 7 13 0.6128 -0.0006 2 7 14 0.7363 -0.0059 2 7 15 0.5059 -0.0042 2 8 0 -3.1691 0.0076 2 8 1 -2.3660 0.0101 2 8 2 -0.6052 0.0089 2 8 3 1.4716 0.0016 2 8 4 3.0845 0.0026 2 8 5 3.8763 0.0131 2 8 6 3.8233 0.0180 2 8 7 2.8942 0.0084 2 8 8 1.3293 -0.0054 2 8 9 -0.0564 -0.0081 2 8 10 -0.5035 -0.0009 2 8 11 -0.1665 0.0020 2 8 12 0.1053 -0.0007 2 8 13 -0.1554 0.0016 2 8 14 -0.5437 0.0089 2 8 15 -0.4983 0.0097 2 9 0 1.5935 0.0306 2 9 1 0.3719 0.0253 2 9 2 -1.2907 0.0142 2 9 3 -2.7104 0.0142 2 9 4 -3.3251 0.0154 2 9 5 -3.1248 0.0095 2 9 6 -2.3855 0.0040 2 9 7 -1.2453 0.0047 2 9 8 0.0325 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-0.2070 0.0085 12 4 0 -0.0209 -0.0015 12 4 1 0.5507 0.0050 12 4 2 0.8216 0.0128 12 4 3 0.8266 0.0107 12 4 4 0.6244 0.0082 12 4 5 0.2521 0.0112 12 4 6 -0.0751 0.0080 12 4 7 -0.3021 -0.0021 12 4 8 -0.6309 -0.0062 12 4 9 -0.9531 -0.0041 12 4 10 -0.8409 -0.0032 12 4 11 -0.2555 -0.0036 12 4 12 0.3221 -0.0065 12 4 13 0.4565 -0.0138 12 4 14 0.1390 -0.0181 12 5 0 -0.4470 0.0020 12 5 1 -0.8571 -0.0047 12 5 2 -0.7889 -0.0132 12 5 3 -0.4328 -0.0078 12 5 4 -0.1021 -0.0003 12 5 5 0.0837 -0.0038 12 5 6 0.1812 -0.0076 12 5 7 0.3812 -0.0041 12 5 8 0.7222 -0.0014 12 5 9 0.8566 -0.0018 12 5 10 0.4809 -0.0019 12 5 11 -0.1894 -0.0012 12 5 12 -0.6439 0.0037 12 5 13 -0.5416 0.0131 12 5 14 0.0244 0.0161 12 5 15 0.5162 0.0083 12 6 0 0.6005 -0.0129 12 6 1 0.7668 -0.0117 12 6 2 0.4853 -0.0038 12 6 3 -0.0170 -0.0109 12 6 4 -0.3690 -0.0224 12 6 5 -0.4238 -0.0178 12 6 6 -0.3643 -0.0047 12 6 7 -0.4678 0.0029 12 6 8 -0.6535 0.0047 12 6 9 -0.5411 0.0043 12 6 10 -0.0552 0.0065 12 6 11 0.4596 0.0127 12 6 12 0.6733 0.0131 12 6 13 0.4382 0.0041 12 6 14 -0.1369 -0.0013 12 6 15 -0.5578 0.0015 12 7 0 -0.5423 0.0148 12 7 1 -0.5097 0.0129 12 7 2 -0.2256 -0.0024 12 7 3 0.2219 -0.0022 12 7 4 0.5858 0.0107 12 7 5 0.6700 0.0140 12 7 6 0.5828 0.0073 12 7 7 0.5549 0.0021 12 7 8 0.4813 0.0032 12 7 9 0.1219 0.0074 12 7 10 -0.3562 0.0045 12 7 11 -0.6115 -0.0081 12 7 12 -0.5929 -0.0143 12 7 13 -0.3363 -0.0081 12 7 14 0.1170 -0.0050 12 7 15 0.4158 -0.0086 12 8 0 0.4287 0.0024 12 8 1 0.2039 0.0065 12 8 2 -0.0213 0.0282 12 8 3 -0.3262 0.0370 12 8 4 -0.6378 0.0260 12 8 5 -0.7358 0.0129 12 8 6 -0.6393 0.0057 12 8 7 -0.5244 0.0019 12 8 8 -0.2817 -0.0038 12 8 9 0.2150 -0.0128 12 8 10 0.6437 -0.0146 12 8 11 0.6971 -0.0061 12 8 12 0.5275 -0.0039 12 8 13 0.2819 -0.0103 12 8 14 -0.0635 -0.0062 12 9 0 -0.2358 -0.0147 12 9 1 0.1798 -0.0029 12 9 2 0.3679 -0.0130 12 9 3 0.4810 -0.0222 12 9 4 0.5884 -0.0185 12 9 5 0.5469 -0.0107 12 9 6 0.4116 -0.0066 12 9 7 0.3347 -0.0086 12 9 8 0.1277 -0.0098 12 9 9 -0.3465 -0.0033 12 9 10 -0.6973 0.0022 12 9 11 -0.6175 0.0024 12 9 12 -0.3591 0.0104 12 9 13 -0.1363 0.0221 12 9 14 0.1099 0.0157 12 10 0 -0.0237 0.0075 12 10 1 -0.4952 -0.0251 12 10 2 -0.6033 -0.0338 12 10 3 -0.5091 -0.0328 12 10 4 -0.3760 -0.0301 12 10 5 -0.1869 -0.0240 12 10 6 -0.0718 -0.0138 12 10 7 -0.1244 0.0013 12 10 8 -0.0369 0.0130 12 10 9 0.3491 0.0137 12 10 10 0.5788 0.0126 12 10 11 0.3525 0.0138 12 10 12 0.0279 0.0044 12 10 13 -0.1151 -0.0099 12 10 14 -0.2021 -0.0079 12 11 0 0.1653 -0.0051 12 11 1 0.4804 0.0105 12 11 2 0.4492 0.0169 12 11 3 0.2442 0.0257 12 11 4 0.0636 0.0301 12 11 5 -0.0627 0.0259 12 11 6 -0.0458 0.0186 12 11 7 0.0859 0.0101 12 11 8 -0.0125 0.0051 12 11 9 -0.3860 0.0061 12 11 10 -0.4875 0.0014 12 11 11 -0.0997 -0.0104 12 11 12 0.2557 -0.0121 12 11 13 0.2561 -0.0048 12 12 0 -0.0784 0.0194 12 12 1 -0.1598 0.0554 12 12 2 -0.0337 0.0673 12 12 3 0.1244 0.0488 12 12 4 0.1388 0.0293 12 12 5 0.0319 0.0204 12 12 6 -0.1399 0.0116 12 12 7 -0.2307 -0.0005 12 12 8 0.0162 -0.0147 12 12 9 0.4488 -0.0272 12 12 10 0.4747 -0.0255 12 12 11 0.0163 -0.0108 12 12 12 -0.2855 -0.0011 12 13 0 -0.0897 -0.0171 12 13 1 -0.1303 -0.0743 12 13 2 -0.2459 -0.0820 12 13 3 -0.3084 -0.0538 12 13 4 -0.1766 -0.0365 12 13 5 0.0863 -0.0376 12 13 6 0.3223 -0.0344 12 13 7 0.3535 -0.0209 12 13 8 0.0444 -0.0031 12 13 9 -0.3651 0.0134 12 13 10 -0.3737 0.0195 12 13 11 -0.0086 0.0153 12 14 3 0.2902 -0.0599 12 14 4 0.1975 -0.0497 12 14 5 -0.0188 -0.0133 12 14 6 -0.2162 0.0113 12 14 7 -0.2760 0.0182 12 14 8 -0.1261 0.0181 12 14 9 0.0995 0.0140 13 -3 2 0.2002 -0.0122 13 -3 3 0.1370 -0.0076 13 -3 4 0.2016 0.0033 13 -3 5 0.3116 0.0132 13 -3 6 0.2715 0.0130 13 -2 0 -0.4471 0.0099 13 -2 1 -0.6021 0.0135 13 -2 2 -0.5697 0.0080 13 -2 3 -0.5189 -0.0013 13 -2 4 -0.5080 -0.0074 13 -2 5 -0.4576 -0.0084 13 -2 6 -0.2189 -0.0044 13 -2 7 0.2451 0.0030 13 -2 8 0.5511 0.0064 13 -1 0 0.4781 -0.0167 13 -1 1 0.5734 -0.0091 13 -1 2 0.6159 0.0037 13 -1 3 0.6962 0.0129 13 -1 4 0.6902 0.0123 13 -1 5 0.4959 0.0070 13 -1 6 0.0619 0.0038 13 -1 7 -0.5480 0.0013 13 -1 8 -0.8384 -0.0011 13 -1 9 -0.3644 -0.0010 13 -1 10 0.3569 -0.0028 13 0 0 -0.2183 0.0061 13 0 1 -0.2272 -0.0021 13 0 2 -0.4057 -0.0084 13 0 3 -0.6520 -0.0103 13 0 4 -0.6378 -0.0065 13 0 5 -0.3222 -0.0036 13 0 6 0.1969 -0.0065 13 0 7 0.8130 -0.0090 13 0 8 1.0356 -0.0062 13 0 9 0.4516 -0.0035 13 0 10 -0.3353 -0.0027 13 0 11 -0.4264 0.0008 13 1 0 0.1012 0.0043 13 1 1 0.0669 0.0049 13 1 2 0.2875 -0.0011 13 1 3 0.4978 -0.0058 13 1 4 0.3496 -0.0063 13 1 5 -0.0049 -0.0026 13 1 6 -0.3802 0.0044 13 1 7 -0.8087 0.0071 13 1 8 -0.9474 0.0028 13 1 9 -0.3945 0.0015 13 1 10 0.3355 0.0078 13 1 11 0.4470 0.0115 13 1 12 0.1386 0.0069 13 2 0 -0.3672 -0.0027 13 2 1 -0.2475 -0.0044 13 2 2 -0.2722 0.0038 13 2 3 -0.2080 0.0082 13 2 4 0.0972 0.0051 13 2 5 0.3038 0.0007 13 2 6 0.3143 -0.0017 13 2 7 0.4427 0.0007 13 2 8 0.5290 0.0076 13 2 9 0.1285 0.0085 13 2 10 -0.4436 -0.0015 13 2 11 -0.5455 -0.0097 13 2 12 -0.3025 -0.0063 13 2 13 -0.1665 -0.0011 13 3 0 0.6329 -0.0024 13 3 1 0.3192 0.0097 13 3 2 0.0442 0.0073 13 3 3 -0.2514 0.0047 13 3 4 -0.5312 0.0068 13 3 5 -0.4469 0.0062 13 3 6 -0.0932 0.0027 13 3 7 0.0213 -0.0009 13 3 8 -0.0295 -0.0065 13 3 9 0.2177 -0.0095 13 3 10 0.5898 -0.0045 13 3 11 0.5900 0.0010 13 3 12 0.3047 -0.0000 13 3 13 0.0928 0.0003 13 4 0 -0.4705 0.0053 13 4 1 0.0274 -0.0090 13 4 2 0.4223 -0.0064 13 4 3 0.6676 -0.0020 13 4 4 0.7414 -0.0032 13 4 5 0.4495 -0.0021 13 4 6 -0.0177 -0.0003 13 4 7 -0.2197 -0.0033 13 4 8 -0.2498 -0.0052 13 4 9 -0.4556 -0.0029 13 4 10 -0.6541 -0.0017 13 4 11 -0.4897 -0.0015 13 4 12 -0.1109 -0.0015 13 4 13 0.1228 -0.0065 13 5 0 0.0447 -0.0064 13 5 1 -0.4697 -0.0008 13 5 2 -0.7432 -0.0094 13 5 3 -0.7717 -0.0158 13 5 4 -0.6677 -0.0107 13 5 5 -0.3831 -0.0067 13 5 6 -0.0444 -0.0060 13 5 7 0.1413 -0.0010 13 5 8 0.2929 0.0052 13 5 9 0.5361 0.0072 13 5 10 0.6190 0.0067 13 5 11 0.3462 0.0043 13 5 12 -0.0489 0.0033 13 5 13 -0.2247 0.0097 13 5 14 -0.0789 0.0164 13 6 0 0.2141 0.0019 13 6 1 0.5813 -0.0017 13 6 2 0.6918 0.0076 13 6 3 0.6045 0.0133 13 6 4 0.4593 0.0043 13 6 5 0.2516 -0.0023 13 6 6 0.0455 0.0019 13 6 7 -0.1031 0.0071 13 6 8 -0.2924 0.0075 13 6 9 -0.4941 0.0037 13 6 10 -0.4906 0.0004 13 6 11 -0.2470 0.0039 13 6 12 0.0305 0.0084 13 6 13 0.1353 0.0020 13 6 14 -0.0306 -0.0081 13 7 0 -0.2615 -0.0003 13 7 1 -0.4144 0.0135 13 7 2 -0.4482 0.0107 13 7 3 -0.3965 0.0039 13 7 4 -0.2521 0.0104 13 7 5 -0.0085 0.0174 13 7 6 0.1879 0.0122 13 7 7 0.2636 0.0005 13 7 8 0.3044 -0.0073 13 7 9 0.2995 -0.0058 13 7 10 0.1933 -0.0026 13 7 11 0.0686 -0.0106 13 7 12 -0.0202 -0.0212 13 7 13 -0.0763 -0.0158 13 7 14 0.0094 -0.0019 13 8 0 0.3351 0.0231 13 8 1 0.2361 -0.0021 13 8 2 0.1909 -0.0079 13 8 3 0.1811 0.0032 13 8 4 0.0157 0.0050 13 8 5 -0.2979 -0.0046 13 8 6 -0.4776 -0.0127 13 8 7 -0.4107 -0.0120 13 8 8 -0.2173 -0.0069 13 8 9 0.0368 -0.0075 13 8 10 0.2561 -0.0094 13 8 11 0.2848 0.0013 13 8 12 0.2079 0.0141 13 8 13 0.1964 0.0095 13 8 14 0.1366 -0.0017 13 9 0 -0.4259 -0.0610 13 9 1 -0.0605 -0.0228 13 9 2 0.1308 -0.0032 13 9 3 0.1464 -0.0157 13 9 4 0.2649 -0.0287 13 9 5 0.4807 -0.0229 13 9 6 0.5130 -0.0052 13 9 7 0.3237 0.0058 13 9 8 0.0483 0.0051 13 9 9 -0.2981 0.0067 13 9 10 -0.5895 0.0116 13 9 11 -0.5905 0.0072 13 9 12 -0.4034 0.0019 13 9 13 -0.2880 0.0104 13 10 0 0.3106 0.0700 13 10 1 -0.1992 0.0116 13 10 2 -0.4783 -0.0261 13 10 3 -0.4645 -0.0191 13 10 4 -0.4279 0.0041 13 10 5 -0.4073 0.0143 13 10 6 -0.2738 0.0089 13 10 7 -0.1187 0.0066 13 10 8 0.0056 0.0139 13 10 9 0.2678 0.0146 13 10 10 0.5691 0.0062 13 10 11 0.5582 0.0028 13 10 12 0.2877 -0.0011 13 10 13 0.0946 -0.0157 13 11 0 -0.0157 -0.0396 13 11 1 0.3912 0.0244 13 11 2 0.5838 0.0640 13 11 3 0.4927 0.0640 13 11 4 0.3377 0.0435 13 11 5 0.1894 0.0246 13 11 6 0.0512 0.0146 13 11 7 0.0582 0.0029 13 11 8 0.1218 -0.0126 13 11 9 -0.0605 -0.0166 13 11 10 -0.3462 -0.0110 13 11 11 -0.2800 -0.0116 13 11 12 0.0708 -0.0115 13 12 1 -0.3064 -0.0133 13 12 2 -0.3354 -0.0236 13 12 3 -0.2211 -0.0279 13 12 4 -0.1139 -0.0292 13 12 5 -0.0527 -0.0270 13 12 6 -0.0469 -0.0252 13 12 7 -0.1683 -0.0205 13 12 8 -0.2466 -0.0137 13 12 9 -0.0208 -0.0145 13 12 10 0.2527 -0.0157 13 12 11 0.1061 -0.0033 13 13 2 0.0011 -0.0681 13 13 3 -0.0492 -0.0595 13 13 4 -0.0322 -0.0363 13 13 5 0.0439 -0.0193 13 13 6 0.1366 -0.0057 13 13 7 0.2445 0.0074 13 13 8 0.2202 0.0193 13 13 9 -0.0658 0.0320 14 -1 2 0.4510 -0.0010 14 -1 3 0.3355 0.0125 14 -1 4 0.2563 0.0138 14 -1 5 0.2647 0.0085 14 -1 6 0.2969 0.0069 14 -1 7 0.1031 0.0072 14 0 0 -0.3568 0.0209 14 0 1 -0.2288 0.0051 14 0 2 -0.1616 -0.0129 14 0 3 -0.2648 -0.0205 14 0 4 -0.3627 -0.0145 14 0 5 -0.3535 -0.0075 14 0 6 -0.2493 -0.0111 14 0 7 0.0740 -0.0179 14 0 8 0.4989 -0.0145 14 0 9 0.4697 -0.0044 14 1 0 0.1345 -0.0080 14 1 1 -0.1202 0.0055 14 1 2 -0.1149 0.0116 14 1 3 0.1602 0.0068 14 1 4 0.2963 -0.0015 14 1 5 0.1778 -0.0012 14 1 6 -0.0067 0.0112 14 1 7 -0.2990 0.0214 14 1 8 -0.6341 0.0152 14 1 9 -0.5265 0.0013 14 1 10 0.0449 -0.0030 14 2 0 -0.1554 0.0128 14 2 1 0.0995 0.0016 14 2 2 0.0926 0.0027 14 2 3 -0.1134 0.0124 14 2 4 -0.0902 0.0166 14 2 5 0.1188 0.0089 14 2 6 0.1940 -0.0051 14 2 7 0.2801 -0.0113 14 2 8 0.5113 -0.0017 14 2 9 0.4734 0.0107 14 2 10 0.0459 0.0074 14 2 11 -0.1988 -0.0062 14 3 0 0.4016 -0.0300 14 3 1 0.1626 -0.0079 14 3 2 0.0465 0.0000 14 3 3 0.0365 -0.0047 14 3 4 -0.1453 -0.0066 14 3 5 -0.2923 -0.0022 14 3 6 -0.1110 0.0024 14 3 7 0.0392 0.0006 14 3 8 -0.1577 -0.0101 14 3 9 -0.2891 -0.0197 14 3 10 -0.0706 -0.0141 14 3 11 0.1163 0.0015 14 3 12 0.0633 0.0088 14 4 0 -0.4737 0.0353 14 4 1 -0.1921 0.0012 14 4 2 0.0418 -0.0172 14 4 3 0.1610 -0.0158 14 4 4 0.3354 -0.0112 14 4 5 0.3341 -0.0084 14 4 6 -0.0333 -0.0049 14 4 7 -0.3022 -0.0015 14 4 8 -0.1293 0.0040 14 4 9 0.0749 0.0104 14 4 10 -0.0195 0.0100 14 4 11 -0.1388 0.0034 14 4 12 -0.0859 -0.0005 14 5 0 0.2349 -0.0290 14 5 1 -0.0867 -0.0020 14 5 2 -0.3133 0.0124 14 5 3 -0.3825 0.0080 14 5 4 -0.4826 0.0030 14 5 5 -0.4340 0.0021 14 5 6 -0.0763 0.0018 14 5 7 0.2115 0.0041 14 5 8 0.1626 0.0069 14 5 9 0.0866 0.0061 14 5 10 0.1950 0.0044 14 5 11 0.2636 0.0025 14 5 12 0.1618 -0.0013 14 6 0 0.0076 0.0242 14 6 1 0.2878 0.0147 14 6 2 0.4343 0.0094 14 6 3 0.4721 0.0159 14 6 4 0.6016 0.0165 14 6 5 0.6235 0.0100 14 6 6 0.3397 0.0056 14 6 7 0.0198 0.0029 14 6 8 -0.1111 -0.0002 14 6 9 -0.2094 -0.0040 14 6 10 -0.3636 -0.0086 14 6 11 -0.4290 -0.0081 14 6 12 -0.3431 0.0004 14 7 0 -0.0543 -0.0224 14 7 1 -0.2114 -0.0156 14 7 2 -0.2933 -0.0052 14 7 3 -0.4060 -0.0071 14 7 4 -0.6318 -0.0073 14 7 5 -0.6673 -0.0022 14 7 6 -0.3517 -0.0011 14 7 7 0.0080 -0.0058 14 7 8 0.1740 -0.0115 14 7 9 0.2495 -0.0104 14 7 10 0.3487 -0.0008 14 7 11 0.4524 0.0027 14 7 12 0.4861 -0.0074 14 8 0 0.0962 0.0315 14 8 1 0.0764 0.0108 14 8 2 0.0696 -0.0200 14 8 3 0.2343 -0.0261 14 8 4 0.4699 -0.0176 14 8 5 0.3971 -0.0117 14 8 6 0.0125 -0.0109 14 8 7 -0.2611 -0.0083 14 8 8 -0.2284 0.0007 14 8 9 -0.0765 0.0067 14 8 10 -0.0301 0.0020 14 8 11 -0.1720 0.0017 14 8 12 -0.3587 0.0145 14 9 0 -0.2787 -0.0656 14 9 1 -0.0583 -0.0324 14 9 2 0.1167 0.0207 14 9 3 0.0239 0.0350 14 9 4 -0.1312 0.0151 14 9 5 0.0118 -0.0026 14 9 6 0.3109 0.0027 14 9 7 0.3509 0.0175 14 9 8 0.0818 0.0186 14 9 9 -0.2444 0.0103 14 9 10 -0.4004 0.0081 14 9 11 -0.2683 0.0040 14 9 12 0.0056 -0.0089 14 10 0 0.3897 0.1020 14 10 1 0.0345 0.0611 14 10 2 -0.2848 -0.0073 14 10 3 -0.2910 -0.0286 14 10 4 -0.1837 -0.0003 14 10 5 -0.2448 0.0291 14 10 6 -0.3155 0.0236 14 10 7 -0.1624 -0.0017 14 10 8 0.1160 -0.0112 14 10 9 0.3717 -0.0054 14 10 10 0.5419 -0.0049 14 10 11 0.4875 -0.0059 14 11 1 0.0913 -0.0423 14 11 2 0.3797 0.0285 14 11 3 0.3916 0.0513 14 11 4 0.2789 0.0211 14 11 5 0.2289 -0.0174 14 11 6 0.1435 -0.0250 14 11 7 -0.0036 -0.0119 14 11 8 -0.0697 -0.0101 14 11 9 -0.1238 -0.0166 14 11 10 -0.2829 -0.0117 14 11 11 -0.3400 -0.0031 14 12 3 -0.2602 -0.0738 14 12 4 -0.1818 -0.0545 14 12 5 -0.1443 -0.0244 14 12 6 -0.0771 -0.0105 14 12 7 -0.0499 -0.0081 14 12 8 -0.1653 0.0022 14 12 9 -0.2104 0.0127 15 1 5 0.1477 -0.0000 15 2 2 0.3608 -0.0026 15 2 3 0.1979 0.0003 15 2 4 -0.0285 0.0092 15 2 5 0.0036 0.0103 15 2 6 0.0777 -0.0039 15 2 7 0.0474 -0.0215 15 2 8 0.1322 -0.0208 15 3 1 -0.0216 -0.0249 15 3 2 -0.2509 -0.0130 15 3 3 -0.1580 -0.0122 15 3 4 -0.0459 -0.0154 15 3 5 -0.1305 -0.0117 15 3 6 -0.1139 0.0001 15 3 7 0.0512 0.0097 15 3 8 -0.0310 0.0045 15 3 9 -0.3204 -0.0117 15 4 1 -0.0773 0.0312 15 4 2 0.1419 0.0032 15 4 3 0.1021 -0.0071 15 4 4 0.0389 -0.0048 15 4 5 0.0806 -0.0016 15 4 6 -0.0637 -0.0007 15 4 7 -0.3106 -0.0004 15 4 8 -0.1678 0.0050 15 4 9 0.2826 0.0155 15 4 10 0.4745 0.0190 15 5 1 -0.0344 -0.0196 15 5 2 -0.1980 0.0140 15 5 3 -0.1058 0.0252 15 5 4 -0.0120 0.0191 15 5 5 -0.0361 0.0098 15 5 6 0.1098 0.0030 15 5 7 0.3440 0.0012 15 5 8 0.2201 0.0010 15 5 9 -0.1700 -0.0037 15 5 10 -0.3198 -0.0087 15 6 1 0.2038 0.0222 15 6 2 0.2850 0.0007 15 6 3 0.1330 -0.0049 15 6 4 0.0819 -0.0005 15 6 5 0.2236 0.0020 15 6 6 0.1886 0.0016 15 6 7 -0.0448 -0.0021 15 6 8 -0.1027 -0.0064 15 6 9 0.0181 -0.0064 15 6 10 0.0108 -0.0049 15 6 11 -0.1358 -0.0043 15 7 1 -0.1823 -0.0389 15 7 2 -0.2026 -0.0262 15 7 3 -0.0941 -0.0193 15 7 4 -0.2086 -0.0170 15 7 5 -0.5050 -0.0124 15 7 6 -0.5168 -0.0077 15 7 7 -0.2008 -0.0042 15 7 8 0.0544 -0.0030 15 7 9 0.1338 -0.0028 15 7 10 0.2123 0.0035 15 7 11 0.3334 0.0126 15 8 1 0.0271 0.0379 15 8 2 -0.0113 0.0133 15 8 3 -0.0376 -0.0057 15 8 4 0.2173 -0.0086 15 8 5 0.5323 -0.0031 15 8 6 0.4558 0.0025 15 8 7 0.0803 0.0048 15 8 8 -0.1617 0.0085 15 8 9 -0.1715 0.0134 15 8 10 -0.1566 0.0073 15 9 2 0.1720 0.0180 15 9 3 0.2017 0.0521 15 9 4 -0.0493 0.0482 15 9 5 -0.2523 0.0218 15 9 6 -0.0922 0.0038 15 9 7 0.1818 0.0059 15 9 8 0.2019 0.0090 15 9 9 0.0097 0.0005 15 9 10 -0.1267 -0.0044 15 10 3 -0.2995 -0.0555 15 10 4 -0.1319 -0.0466 15 10 5 -0.0266 -0.0068 15 10 6 -0.1428 0.0129 15 10 7 -0.2082 -0.0052 15 10 8 -0.0462 -0.0257 15 10 9 0.1941 -0.0210 15 11 6 0.1071 -0.0399 15 11 7 0.0430 -0.0155 0 0 0 0.0 0.0 ; _shelx_fab_checksum 8624 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.09905(3) -0.11528(3) 0.94540(3) 0.08048(16) Uani 1 1 d . . . . . O1 O 0.56047(17) 0.28325(17) 0.38919(18) 0.0661(5) Uani 1 1 d . . . . . N4 N 0.11608(18) 0.26495(17) 0.70125(17) 0.0471(5) Uani 1 1 d . . . . . N3 N 0.4095(2) 0.40264(19) 0.58475(19) 0.0499(5) Uani 1 1 d . . . . . N2 N 0.3703(2) 0.57275(18) 0.33724(19) 0.0511(5) Uani 1 1 d . . . . . N1 N 0.4670(2) 0.46713(18) 0.30418(18) 0.0510(5) Uani 1 1 d . . . . . C31 C 0.2286(2) 0.2012(2) 0.65828(19) 0.0411(5) Uani 1 1 d . . . . . C16 C 0.2750(2) 0.3654(2) 0.5137(2) 0.0407(5) Uani 1 1 d . . . . . H16 H 0.196984 0.417491 0.556058 0.049 Uiso 1 1 calc R U . . . C35 C 0.1287(2) 0.0683(2) 0.7507(2) 0.0459(6) Uani 1 1 d . . . . . C8 C 0.3722(2) 0.4274(2) 0.4863(2) 0.0441(5) Uani 1 1 d . . . . . C36 C 0.0517(2) 0.1861(2) 0.7589(2) 0.0461(6) Uani 1 1 d . . . . . C23 C 0.3225(2) 0.2574(2) 0.59333(19) 0.0412(5) Uani 1 1 d . . . . . H23 H 0.396372 0.198769 0.553363 0.049 Uiso 1 1 calc R U . . . C7 C 0.4798(2) 0.3801(2) 0.3887(2) 0.0491(6) Uani 1 1 d . . . . . C40 C 0.0846(2) -0.0223(2) 0.8049(2) 0.0538(6) Uani 1 1 d . . . . . H40 H 0.135310 -0.101111 0.800401 0.065 Uiso 1 1 calc R U . . . C9 C 0.3201(2) 0.5542(2) 0.4392(2) 0.0424(5) Uani 1 1 d . . . . . C10 C 0.2175(2) 0.6492(2) 0.4974(2) 0.0468(6) Uani 1 1 d . . . . . C18 C 0.2490(2) 0.3466(2) 0.4178(2) 0.0442(5) Uani 1 1 d . . . . . C32 C 0.2542(2) 0.0678(2) 0.6799(2) 0.0463(6) Uani 1 1 d . . . . . C38 C -0.1152(3) 0.1242(3) 0.8730(2) 0.0627(8) Uani 1 1 d . . . . . H38 H -0.197300 0.141411 0.914288 0.075 Uiso 1 1 calc R U . . . C24 C 0.3592(2) 0.3144(2) 0.6627(2) 0.0468(6) Uani 1 1 d . . . . . H24 H 0.283434 0.357317 0.714554 0.056 Uiso 1 1 calc R U . . . C37 C -0.0709(3) 0.2150(3) 0.8186(2) 0.0599(7) Uani 1 1 d . . . . . H37 H -0.122351 0.293699 0.822196 0.072 Uiso 1 1 calc R U . . . C39 C -0.0380(3) 0.0082(3) 0.8663(2) 0.0559(7) Uani 1 1 d . . . . . C34 C 0.2885(3) 0.0176(3) 0.5735(3) 0.0644(8) Uani 1 1 d . . . . . H34A H 0.226402 0.062309 0.536309 0.097 Uiso 1 1 calc R U . . . H34B H 0.293778 -0.063715 0.589470 0.097 Uiso 1 1 calc R U . . . H34C H 0.366935 0.022716 0.528168 0.097 Uiso 1 1 calc R U . . . C17 C 0.1476(2) 0.4285(3) 0.3843(2) 0.0558(7) Uani 1 1 d . . . . . H17 H 0.097113 0.493508 0.421844 0.067 Uiso 1 1 calc R U . . . C25 C 0.4464(3) 0.2303(2) 0.7258(2) 0.0571(7) Uani 1 1 d . . . . . C15 C 0.1919(3) 0.6472(2) 0.6083(3) 0.0602(7) Uani 1 1 d . . . . . H15 H 0.239082 0.584081 0.647506 0.072 Uiso 1 1 calc R U . . . C33 C 0.3539(3) -0.0006(2) 0.7393(3) 0.0662(8) Uani 1 1 d . . . . . H33A H 0.430982 0.008275 0.694668 0.099 Uiso 1 1 calc R U . . . H33B H 0.363134 -0.082945 0.753479 0.099 Uiso 1 1 calc R U . . . H33C H 0.330033 0.029943 0.806856 0.099 Uiso 1 1 calc R U . . . C19 C 0.3236(3) 0.2521(2) 0.3586(2) 0.0584(7) Uani 1 1 d . . . . . H19 H 0.392629 0.197083 0.378945 0.070 Uiso 1 1 calc R U . . . C4 C 0.5434(3) 0.4698(3) 0.1959(2) 0.0617(7) Uani 1 1 d . . . . . C11 C 0.1457(3) 0.7437(3) 0.4410(3) 0.0690(8) Uani 1 1 d . . . . . H11 H 0.161656 0.746702 0.366371 0.083 Uiso 1 1 calc R U . . . C20 C 0.2974(4) 0.2381(3) 0.2703(3) 0.0731(9) Uani 1 1 d . . . . . H20 H 0.348240 0.174327 0.231203 0.088 Uiso 1 1 calc R U . . . C26 C 0.5667(3) 0.1670(3) 0.6743(3) 0.0753(9) Uani 1 1 d . . . . . H26 H 0.595366 0.176763 0.598732 0.090 Uiso 1 1 calc R U . . . C14 C 0.0957(3) 0.7394(3) 0.6612(3) 0.0779(10) Uani 1 1 d . . . . . H14 H 0.079193 0.738093 0.735672 0.093 Uiso 1 1 calc R U . . . C3 C 0.5158(4) 0.5688(3) 0.1231(3) 0.0788(10) Uani 1 1 d . . . . . H3A H 0.446739 0.634744 0.144934 0.095 Uiso 1 1 calc R U . . . C30 C 0.4066(4) 0.2134(3) 0.8382(3) 0.0804(10) Uani 1 1 d . . . . . H30 H 0.325979 0.255932 0.874249 0.096 Uiso 1 1 calc R U . . . C22 C 0.1208(3) 0.4147(4) 0.2964(3) 0.0756(9) Uani 1 1 d . . . . . H22 H 0.052402 0.469993 0.275173 0.091 Uiso 1 1 calc R U . . . C13 C 0.0264(3) 0.8305(3) 0.6053(4) 0.0857(11) Uani 1 1 d . . . . . H13 H -0.037864 0.891649 0.641445 0.103 Uiso 1 1 calc R U . . . C21 C 0.1944(4) 0.3202(4) 0.2405(3) 0.0812(10) Uani 1 1 d . . . . . H21 H 0.175255 0.310773 0.181719 0.097 Uiso 1 1 calc R U . . . C12 C 0.0498(3) 0.8339(3) 0.4961(4) 0.0882(11) Uani 1 1 d . . . . . H12 H 0.001105 0.897191 0.458252 0.106 Uiso 1 1 calc R U . . . C27 C 0.6451(4) 0.0887(3) 0.7353(6) 0.1113(18) Uani 1 1 d . . . . . H27 H 0.726731 0.047576 0.700427 0.134 Uiso 1 1 calc R U . . . C2 C 0.5903(5) 0.5711(4) 0.0172(3) 0.1017(14) Uani 1 1 d . . . . . H2 H 0.571035 0.638748 -0.032131 0.122 Uiso 1 1 calc R U . . . C28 C 0.6034(7) 0.0720(4) 0.8451(7) 0.131(2) Uani 1 1 d . . . . . H28 H 0.655652 0.017790 0.885363 0.157 Uiso 1 1 calc R U . . . C5 C 0.6467(4) 0.3721(4) 0.1640(3) 0.0958(13) Uani 1 1 d . . . . . H5 H 0.666126 0.304339 0.213127 0.115 Uiso 1 1 calc R U . . . C1 C 0.6913(5) 0.4757(4) -0.0154(4) 0.1157(17) Uani 1 1 d . . . . . H1 H 0.740419 0.477192 -0.087169 0.139 Uiso 1 1 calc R U . . . C29 C 0.4846(7) 0.1346(4) 0.8971(5) 0.122(2) Uani 1 1 d . . . . . H29 H 0.456535 0.123601 0.972648 0.147 Uiso 1 1 calc R U . . . C6 C 0.7207(5) 0.3769(5) 0.0576(4) 0.1222(18) Uani 1 1 d . . . . . H6 H 0.791315 0.312249 0.035608 0.147 Uiso 1 1 calc R U . . . H3 H 0.485(3) 0.381(3) 0.569(2) 0.053(8) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0764(3) 0.0862(3) 0.0811(3) 0.00489(18) -0.01018(18) -0.0494(2) O1 0.0458(10) 0.0465(11) 0.0843(14) -0.0144(10) -0.0046(10) -0.0021(9) N4 0.0388(11) 0.0411(11) 0.0525(12) -0.0104(9) -0.0053(9) -0.0086(9) N3 0.0460(13) 0.0407(11) 0.0669(15) -0.0029(10) -0.0248(11) -0.0134(10) N2 0.0469(12) 0.0397(11) 0.0612(14) -0.0071(10) -0.0090(10) -0.0142(9) N1 0.0462(12) 0.0435(11) 0.0563(13) -0.0123(10) -0.0025(10) -0.0151(10) C31 0.0381(12) 0.0382(12) 0.0439(13) -0.0081(10) -0.0100(10) -0.0096(10) C16 0.0341(11) 0.0348(11) 0.0495(13) -0.0072(10) -0.0096(10) -0.0089(9) C35 0.0417(13) 0.0431(13) 0.0504(14) -0.0086(11) -0.0106(11) -0.0125(11) C8 0.0375(12) 0.0361(12) 0.0564(15) -0.0073(10) -0.0124(11) -0.0103(10) C36 0.0404(13) 0.0465(13) 0.0454(13) -0.0101(11) -0.0059(10) -0.0117(11) C23 0.0353(11) 0.0357(11) 0.0476(13) -0.0086(10) -0.0091(10) -0.0074(10) C7 0.0395(13) 0.0432(14) 0.0630(16) -0.0101(12) -0.0088(11) -0.0153(12) C40 0.0504(15) 0.0484(14) 0.0612(17) -0.0064(12) -0.0128(13) -0.0183(12) C9 0.0375(12) 0.0361(12) 0.0544(15) -0.0087(10) -0.0126(11) -0.0120(10) C10 0.0387(13) 0.0349(12) 0.0645(17) -0.0085(11) -0.0117(12) -0.0114(10) C18 0.0428(13) 0.0428(13) 0.0486(14) -0.0026(10) -0.0111(11) -0.0196(11) C32 0.0382(12) 0.0369(12) 0.0580(15) -0.0081(11) -0.0069(11) -0.0114(10) C38 0.0449(15) 0.082(2) 0.0573(17) -0.0176(15) 0.0020(12) -0.0263(15) C24 0.0439(13) 0.0405(13) 0.0539(15) -0.0084(11) -0.0149(11) -0.0101(11) C37 0.0459(15) 0.0587(17) 0.0620(17) -0.0159(13) -0.0012(13) -0.0120(13) C39 0.0539(16) 0.0631(17) 0.0536(16) -0.0052(13) -0.0095(12) -0.0289(14) C34 0.0618(18) 0.0500(16) 0.0725(19) -0.0230(14) 0.0043(15) -0.0211(14) C17 0.0448(14) 0.0611(17) 0.0609(17) -0.0016(13) -0.0155(13) -0.0207(13) C25 0.0668(18) 0.0436(14) 0.0731(19) 0.0038(13) -0.0382(15) -0.0219(13) C15 0.0574(17) 0.0457(15) 0.0684(19) -0.0149(13) -0.0101(14) -0.0104(13) C33 0.0498(16) 0.0425(14) 0.100(2) 0.0043(14) -0.0257(16) -0.0132(13) C19 0.0684(18) 0.0480(15) 0.0594(17) -0.0077(12) -0.0196(14) -0.0187(14) C4 0.0638(18) 0.0599(17) 0.0617(18) -0.0172(14) 0.0017(14) -0.0326(15) C11 0.0628(18) 0.0495(17) 0.085(2) -0.0056(15) -0.0258(17) -0.0066(15) C20 0.102(3) 0.068(2) 0.0584(19) -0.0133(15) -0.0168(18) -0.041(2) C26 0.0564(18) 0.0510(17) 0.119(3) 0.0085(17) -0.0405(19) -0.0161(15) C14 0.075(2) 0.060(2) 0.084(2) -0.0293(17) 0.0014(18) -0.0166(18) C3 0.094(3) 0.065(2) 0.067(2) -0.0120(16) 0.0010(18) -0.0351(19) C30 0.115(3) 0.066(2) 0.075(2) 0.0045(17) -0.049(2) -0.035(2) C22 0.069(2) 0.096(3) 0.070(2) 0.0067(19) -0.0356(17) -0.034(2) C13 0.058(2) 0.053(2) 0.123(3) -0.032(2) 0.001(2) -0.0055(16) C21 0.103(3) 0.103(3) 0.065(2) -0.002(2) -0.035(2) -0.059(3) C12 0.066(2) 0.0500(18) 0.128(4) -0.011(2) -0.033(2) 0.0056(16) C27 0.080(3) 0.060(2) 0.207(6) 0.028(3) -0.084(3) -0.025(2) C2 0.139(4) 0.087(3) 0.068(2) -0.009(2) 0.005(2) -0.058(3) C28 0.169(6) 0.075(3) 0.205(6) 0.058(4) -0.151(6) -0.059(3) C5 0.086(3) 0.080(2) 0.078(2) -0.0203(19) 0.016(2) -0.012(2) C1 0.137(4) 0.106(3) 0.079(3) -0.035(3) 0.039(3) -0.061(3) C29 0.209(6) 0.085(3) 0.118(4) 0.038(3) -0.112(4) -0.069(4) C6 0.114(4) 0.107(3) 0.091(3) -0.030(3) 0.030(3) -0.022(3) 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' Br Br -0.2901 2.4595 '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' 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 C31 N4 C36 106.94(19) . . ? C8 N3 C24 109.8(2) . . ? C8 N3 H3 110(2) . . ? C24 N3 H3 113(2) . . ? C9 N2 N1 108.2(2) . . ? C7 N1 N2 112.0(2) . . ? C7 N1 C4 129.4(2) . . ? C4 N1 N2 118.2(2) . . ? N4 C31 C23 120.7(2) . . ? N4 C31 C32 114.6(2) . . ? C23 C31 C32 124.69(19) . . ? C8 C16 H16 106.5 . . ? C23 C16 H16 106.5 . . ? C23 C16 C8 101.95(18) . . ? C18 C16 H16 106.5 . . ? C18 C16 C8 115.7(2) . . ? C18 C16 C23 118.68(19) . . ? C36 C35 C32 107.7(2) . . ? C40 C35 C36 120.5(2) . . ? C40 C35 C32 131.8(2) . . ? N3 C8 C16 105.1(2) . . ? N3 C8 C7 112.8(2) . . ? N3 C8 C9 119.0(2) . . ? C7 C8 C16 110.31(19) . . ? C9 C8 C16 109.68(19) . . ? C9 C8 C7 100.0(2) . . ? C35 C36 N4 111.6(2) . . ? C37 C36 N4 127.2(2) . . ? C37 C36 C35 121.2(2) . . ? C31 C23 C16 113.48(19) . . ? C31 C23 H23 109.7 . . ? C31 C23 C24 113.6(2) . . ? C16 C23 H23 109.7 . . ? C16 C23 C24 100.41(18) . . ? C24 C23 H23 109.7 . . ? O1 C7 N1 128.0(3) . . ? O1 C7 C8 125.7(3) . . ? N1 C7 C8 106.3(2) . . ? C35 C40 H40 121.2 . . ? C35 C40 C39 117.5(2) . . ? C39 C40 H40 121.2 . . ? N2 C9 C8 112.8(2) . . ? N2 C9 C10 120.7(2) . . ? C10 C9 C8 126.4(2) . . ? C15 C10 C9 121.1(2) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 C15 118.9(2) . . ? C17 C18 C16 119.1(2) . . ? C19 C18 C16 122.9(2) . . ? C19 C18 C17 118.0(2) . . ? C31 C32 C34 110.6(2) . . ? C31 C32 C33 113.3(2) . . ? C35 C32 C31 99.12(18) . . ? C35 C32 C34 111.4(2) . . ? C35 C32 C33 111.8(2) . . ? C34 C32 C33 110.3(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C39 C38 C37 120.1(3) . . ? N3 C24 C23 104.9(2) . . ? N3 C24 H24 107.8 . . ? N3 C24 C25 112.5(2) . . ? C23 C24 H24 107.8 . . ? C25 C24 C23 115.7(2) . . ? C25 C24 H24 107.8 . . ? C36 C37 C38 118.3(3) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C40 C39 Br1 118.2(2) . . ? C38 C39 Br1 119.5(2) . . ? C38 C39 C40 122.3(3) . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C17 H17 119.5 . . ? C22 C17 C18 121.0(3) . . ? C22 C17 H17 119.5 . . ? C26 C25 C24 121.4(3) . . ? C26 C25 C30 118.6(3) . . ? C30 C25 C24 120.0(3) . . ? C10 C15 H15 120.0 . . ? C10 C15 C14 120.0(3) . . ? C14 C15 H15 120.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C18 C19 H19 119.3 . . ? C20 C19 C18 121.3(3) . . ? C20 C19 H19 119.3 . . ? C3 C4 N1 120.2(3) . . ? C3 C4 C5 120.1(3) . . ? C5 C4 N1 119.8(3) . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.8(3) . . ? C12 C11 H11 120.1 . . ? C19 C20 H20 120.5 . . ? C19 C20 C21 119.1(3) . . ? C21 C20 H20 120.5 . . ? C25 C26 H26 120.0 . . ? C25 C26 C27 120.0(4) . . ? C27 C26 H26 120.0 . . ? C15 C14 H14 119.8 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C4 C3 H3A 119.9 . . ? C4 C3 C2 120.1(3) . . ? C2 C3 H3A 119.9 . . ? C25 C30 H30 119.7 . . ? C29 C30 C25 120.7(5) . . ? C29 C30 H30 119.7 . . ? C17 C22 H22 120.0 . . ? C21 C22 C17 120.0(3) . . ? C21 C22 H22 120.0 . . ? C14 C13 H13 119.8 . . ? C14 C13 C12 120.5(3) . . ? C12 C13 H13 119.8 . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21 119.7 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C26 C27 H27 119.8 . . ? C28 C27 C26 120.4(5) . . ? C28 C27 H27 119.8 . . ? C3 C2 H2 119.8 . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C27 C28 H28 119.9 . . ? C27 C28 C29 120.1(4) . . ? C29 C28 H28 119.9 . . ? C4 C5 H5 120.6 . . ? C4 C5 C6 118.8(4) . . ? C6 C5 H5 120.6 . . ? C2 C1 H1 120.1 . . ? C2 C1 C6 119.7(4) . . ? C6 C1 H1 120.1 . . ? C30 C29 H29 119.9 . . ? C28 C29 C30 120.2(5) . . ? C28 C29 H29 119.9 . . ? C5 C6 H6 119.6 . . ? C1 C6 C5 120.8(4) . . ? C1 C6 H6 119.6 . . ? 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 Br1 C39 1.897(3) . ? O1 C7 1.216(3) . ? N4 C31 1.289(3) . ? N4 C36 1.415(3) . ? N3 C8 1.449(3) . ? N3 C24 1.479(3) . ? N3 H3 0.82(3) . ? N2 N1 1.414(3) . ? N2 C9 1.277(3) . ? N1 C7 1.354(3) . ? N1 C4 1.412(4) . ? C31 C23 1.490(3) . ? C31 C32 1.530(3) . ? C16 H16 0.9800 . ? C16 C8 1.566(3) . ? C16 C23 1.535(3) . ? C16 C18 1.499(3) . ? C35 C36 1.395(3) . ? C35 C40 1.376(4) . ? C35 C32 1.500(3) . ? C8 C7 1.523(4) . ? C8 C9 1.505(3) . ? C36 C37 1.380(4) . ? C23 H23 0.9800 . ? C23 C24 1.551(3) . ? C40 H40 0.9300 . ? C40 C39 1.385(4) . ? C9 C10 1.468(3) . ? C10 C15 1.382(4) . ? C10 C11 1.382(4) . ? C18 C17 1.391(4) . ? C18 C19 1.385(4) . ? C32 C34 1.531(4) . ? C32 C33 1.532(4) . ? C38 H38 0.9300 . ? C38 C37 1.381(4) . ? C38 C39 1.377(4) . ? C24 H24 0.9800 . ? C24 C25 1.495(4) . ? C37 H37 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C17 H17 0.9300 . ? C17 C22 1.375(4) . ? C25 C26 1.379(4) . ? C25 C30 1.382(5) . ? C15 H15 0.9300 . ? C15 C14 1.391(4) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C19 H19 0.9300 . ? C19 C20 1.379(4) . ? C4 C3 1.365(5) . ? C4 C5 1.382(5) . ? C11 H11 0.9300 . ? C11 C12 1.387(5) . ? C20 H20 0.9300 . ? C20 C21 1.384(5) . ? C26 H26 0.9300 . ? C26 C27 1.389(5) . ? C14 H14 0.9300 . ? C14 C13 1.344(5) . ? C3 H3A 0.9300 . ? C3 C2 1.381(5) . ? C30 H30 0.9300 . ? C30 C29 1.370(6) . ? C22 H22 0.9300 . ? C22 C21 1.361(5) . ? C13 H13 0.9300 . ? C13 C12 1.361(6) . ? C21 H21 0.9300 . ? C12 H12 0.9300 . ? C27 H27 0.9300 . ? C27 C28 1.352(8) . ? C2 H2 0.9300 . ? C2 C1 1.355(6) . ? C28 H28 0.9300 . ? C28 C29 1.366(9) . ? C5 H5 0.9300 . ? C5 C6 1.385(5) . ? C1 H1 0.9300 . ? C1 C6 1.369(7) . ? C29 H29 0.9300 . ? C6 H6 0.9300 . ? 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 N4 C31 C23 C16 -44.0(3) . . . . ? N4 C31 C23 C24 69.9(3) . . . . ? N4 C31 C32 C35 -2.1(3) . . . . ? N4 C31 C32 C34 114.9(3) . . . . ? N4 C31 C32 C33 -120.7(3) . . . . ? N4 C36 C37 C38 -177.3(3) . . . . ? N3 C8 C7 O1 43.6(3) . . . . ? N3 C8 C7 N1 -135.8(2) . . . . ? N3 C8 C9 N2 131.3(2) . . . . ? N3 C8 C9 C10 -52.6(3) . . . . ? N3 C24 C25 C26 -53.7(3) . . . . ? N3 C24 C25 C30 127.2(3) . . . . ? N2 N1 C7 O1 -172.8(3) . . . . ? N2 N1 C7 C8 6.6(3) . . . . ? N2 N1 C4 C3 -6.4(4) . . . . ? N2 N1 C4 C5 173.0(3) . . . . ? N2 C9 C10 C15 -156.2(3) . . . . ? N2 C9 C10 C11 22.9(4) . . . . ? N1 N2 C9 C8 -4.7(3) . . . . ? N1 N2 C9 C10 178.9(2) . . . . ? N1 C4 C3 C2 -179.8(3) . . . . ? N1 C4 C5 C6 -179.5(4) . . . . ? C31 N4 C36 C35 0.0(3) . . . . ? C31 N4 C36 C37 179.1(3) . . . . ? C31 C23 C24 N3 -158.0(2) . . . . ? C31 C23 C24 C25 77.5(3) . . . . ? C16 C8 C7 O1 -73.5(3) . . . . ? C16 C8 C7 N1 107.1(2) . . . . ? C16 C8 C9 N2 -107.8(2) . . . . ? C16 C8 C9 C10 68.4(3) . . . . ? C16 C23 C24 N3 -36.5(2) . . . . ? C16 C23 C24 C25 -161.0(2) . . . . ? C16 C18 C17 C22 179.7(3) . . . . ? C16 C18 C19 C20 -179.5(3) . . . . ? C35 C36 C37 C38 1.8(4) . . . . ? C35 C40 C39 Br1 -178.0(2) . . . . ? C35 C40 C39 C38 0.8(4) . . . . ? C8 N3 C24 C23 17.0(3) . . . . ? C8 N3 C24 C25 143.5(2) . . . . ? C8 C16 C23 C31 162.85(19) . . . . ? C8 C16 C23 C24 41.2(2) . . . . ? C8 C16 C18 C17 -96.2(3) . . . . ? C8 C16 C18 C19 82.2(3) . . . . ? C8 C9 C10 C15 28.0(4) . . . . ? C8 C9 C10 C11 -152.9(3) . . . . ? C36 N4 C31 C23 -178.7(2) . . . . ? C36 N4 C31 C32 1.4(3) . . . . ? C36 C35 C40 C39 0.5(4) . . . . ? C36 C35 C32 C31 1.9(3) . . . . ? C36 C35 C32 C34 -114.5(2) . . . . ? C36 C35 C32 C33 121.6(2) . . . . ? C23 C31 C32 C35 178.0(2) . . . . ? C23 C31 C32 C34 -65.0(3) . . . . ? C23 C31 C32 C33 59.4(3) . . . . ? C23 C16 C8 N3 -32.4(2) . . . . ? C23 C16 C8 C7 89.4(2) . . . . ? C23 C16 C8 C9 -161.4(2) . . . . ? C23 C16 C18 C17 142.1(2) . . . . ? C23 C16 C18 C19 -39.5(3) . . . . ? C23 C24 C25 C26 66.8(3) . . . . ? C23 C24 C25 C30 -112.2(3) . . . . ? C7 N1 C4 C3 -178.0(3) . . . . ? C7 N1 C4 C5 1.5(5) . . . . ? C7 C8 C9 N2 8.2(3) . . . . ? C7 C8 C9 C10 -175.7(2) . . . . ? C40 C35 C36 N4 177.4(2) . . . . ? C40 C35 C36 C37 -1.9(4) . . . . ? C40 C35 C32 C31 -176.6(3) . . . . ? C40 C35 C32 C34 67.0(4) . . . . ? C40 C35 C32 C33 -56.9(4) . . . . ? C9 N2 N1 C7 -1.4(3) . . . . ? C9 N2 N1 C4 -174.3(2) . . . . ? C9 C8 C7 O1 171.1(3) . . . . ? C9 C8 C7 N1 -8.3(2) . . . . ? C9 C10 C15 C14 178.7(3) . . . . ? C9 C10 C11 C12 -179.2(3) . . . . ? C10 C15 C14 C13 0.5(5) . . . . ? C10 C11 C12 C13 0.5(6) . . . . ? C18 C16 C8 N3 -162.7(2) . . . . ? C18 C16 C8 C7 -40.9(3) . . . . ? C18 C16 C8 C9 68.3(3) . . . . ? C18 C16 C23 C31 -68.7(3) . . . . ? C18 C16 C23 C24 169.7(2) . . . . ? C18 C17 C22 C21 -0.3(5) . . . . ? C18 C19 C20 C21 -0.1(5) . . . . ? C32 C31 C23 C16 135.9(2) . . . . ? C32 C31 C23 C24 -110.2(3) . . . . ? C32 C35 C36 N4 -1.3(3) . . . . ? C32 C35 C36 C37 179.5(2) . . . . ? C32 C35 C40 C39 178.8(3) . . . . ? C24 N3 C8 C16 9.5(3) . . . . ? C24 N3 C8 C7 -110.7(2) . . . . ? C24 N3 C8 C9 132.8(2) . . . . ? C24 C25 C26 C27 -179.4(3) . . . . ? C24 C25 C30 C29 178.5(3) . . . . ? C37 C38 C39 Br1 177.9(2) . . . . ? C37 C38 C39 C40 -0.8(5) . . . . ? C39 C38 C37 C36 -0.5(5) . . . . ? C17 C18 C19 C20 -1.0(4) . . . . ? C17 C22 C21 C20 -0.8(6) . . . . ? C25 C26 C27 C28 1.5(6) . . . . ? C25 C30 C29 C28 0.4(6) . . . . ? C15 C10 C11 C12 -0.2(5) . . . . ? C15 C14 C13 C12 -0.2(6) . . . . ? C19 C18 C17 C22 1.3(4) . . . . ? C19 C20 C21 C22 1.0(5) . . . . ? C4 N1 C7 O1 -0.9(5) . . . . ? C4 N1 C7 C8 178.5(3) . . . . ? C4 C3 C2 C1 -0.1(7) . . . . ? C4 C5 C6 C1 -1.2(8) . . . . ? C11 C10 C15 C14 -0.3(4) . . . . ? C26 C25 C30 C29 -0.6(5) . . . . ? C26 C27 C28 C29 -1.8(7) . . . . ? C14 C13 C12 C11 -0.3(6) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C3 C2 C1 C6 -1.1(8) . . . . ? C30 C25 C26 C27 -0.3(5) . . . . ? C27 C28 C29 C30 0.9(7) . . . . ? C2 C1 C6 C5 1.7(9) . . . . ? C5 C4 C3 C2 0.7(6) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.500 1.000 136.6 33.7 ? 2 0.405 0.819 0.936 23.1 0.0 ? 3 0.595 0.181 0.064 23.1 0.0 ?