#------------------------------------------------------------------------------ #$Date: 2024-10-18 00:52:07 +0300 (Fri, 18 Oct 2024) $ #$Revision: 295521 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572880.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_1572880 _journal_paper_doi 10.1039/D4CC04720F _chemical_formula_moiety 'C26 H20 Br N O4' _chemical_formula_sum 'C26 H20 Br N O4' _chemical_formula_weight 490.34 _chemical_name_systematic 2-(4-bromobenzoyel)-3-(4-dimethylamio)phenyl)-2,3-dihydro-4H-furo[3,2-c]chromen-4-one _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 geom _atom_sites_solution_primary iterative _audit_creation_date 2023-04-15 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2024-07-01 deposited with the CCDC. 2024-10-17 downloaded from the CCDC. ; _cell_angle_alpha 82.4456(10) _cell_angle_beta 83.3581(12) _cell_angle_gamma 85.9012(11) _cell_formula_units_Z 2 _cell_length_a 5.03990(8) _cell_length_b 14.26675(16) _cell_length_c 15.1370(2) _cell_measurement_reflns_used 13185 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 68.2450 _cell_measurement_theta_min 2.9540 _cell_volume 1069.96(3) _computing_cell_refinement 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -26.00 43.00 0.50 0.20 -- 40.33 -38.00 90.00 138 2 \w -26.00 57.00 0.50 0.20 -- 40.33 -50.00 0.00 166 3 \w -35.00 24.00 0.50 0.20 -- 40.33 -12.00 -60.00 118 4 \w -30.00 31.00 0.50 0.20 -- 40.33 -25.00-180.00 122 5 \w -35.00 24.00 0.50 0.20 -- 40.33 -12.00-150.00 118 6 \w -35.00 24.00 0.50 0.20 -- 40.33 -12.00-120.00 118 7 \w 12.00 43.00 0.50 0.20 -- 40.33 81.00 122.65 62 8 \w 9.00 43.00 0.50 0.20 -- 40.33 90.00 170.73 68 9 \w 14.00 109.00 0.50 0.20 -- 40.33 77.00 60.00 190 10 \w 14.00 109.00 0.50 0.20 -- 40.33 77.00 150.00 190 11 \w 14.00 109.00 0.50 0.20 -- 40.33 77.00 0.00 190 12 \w 14.00 109.00 0.50 0.20 -- 40.33 77.00 -90.00 190 13 \w 11.00 43.00 0.50 0.20 -- 40.33 85.00 -48.43 64 14 \w 83.00 164.00 0.50 0.20 -- 96.67 33.00-180.00 162 15 \w 78.00 163.00 0.50 0.20 -- 96.67 50.00-150.00 170 16 \w 78.00 163.00 0.50 0.20 -- 96.67 50.00 -30.00 170 17 \w 75.00 164.00 0.50 0.20 -- 96.67 59.00 30.00 178 18 \w 78.00 163.00 0.50 0.20 -- 96.67 50.00 90.00 170 19 \w 73.00 165.00 0.50 0.20 -- 96.67 68.00 120.00 184 20 \w 74.00 162.00 0.50 0.20 -- 96.67 155.00 19.00 176 21 \w 105.00 170.00 0.50 0.20 -- 96.67 96.00 -90.00 130 22 \w 97.00 163.00 0.50 0.20 -- 96.67 121.00-138.00 132 23 \w 81.00 164.00 0.50 0.20 -- 96.67 145.00-180.00 166 24 \w 99.00 164.00 0.50 0.20 -- 96.67 117.00-150.00 130 25 \w 30.00 57.00 0.50 0.20 -- 96.67 -50.00-120.00 54 26 \w 29.00 68.00 0.50 0.20 -- 96.67 -59.00-180.00 78 27 \w 29.00 83.00 0.50 0.20 -- 96.67 -68.00-150.00 108 28 \w 28.00 105.00 0.50 0.20 -- 96.67 -77.00 -30.00 154 29 \w 29.00 68.00 0.50 0.20 -- 96.67 -59.00 30.00 78 30 \w 29.00 83.00 0.50 0.20 -- 96.67 -68.00 150.00 108 31 \w 27.00 127.00 0.50 0.20 -- 96.67 -87.00 120.00 200 32 \w 31.00 111.00 0.50 0.20 -- 96.67-121.00 138.00 160 33 \w 44.00 127.00 0.50 0.20 -- 96.67-145.00 60.00 166 34 \w 30.00 109.00 0.50 0.20 -- 96.67-117.00 60.00 158 35 \w 49.00 133.00 0.50 0.20 -- 96.67-155.00 -18.00 168 36 \w 30.00 109.00 0.50 0.20 -- 96.67-117.00 -30.00 158 37 \w 44.00 127.00 0.50 0.20 -- 96.67-145.00 -60.00 166 38 \w 22.00 106.00 0.50 0.20 -- 96.67 -96.00 -30.00 168 39 \w 30.00 109.00 0.50 0.20 -- 96.67-117.00-150.00 158 40 \w 49.00 110.00 0.50 0.20 -- 40.33-155.00 -18.00 122 41 \w 31.00 88.00 0.50 0.20 -- 40.33-121.00 138.00 114 42 \w -110.00 -26.00 0.50 0.20 -- -40.33 -25.00 -60.00 168 43 \w -108.00 -17.00 0.50 0.20 -- -40.33 -64.00-150.00 182 44 \w -107.00 -21.00 0.50 0.20 -- -40.33 -50.00 -90.00 172 45 \w -106.00 -25.00 0.50 0.20 -- -40.33 -38.00-150.00 162 46 \w -107.00 -21.00 0.50 0.20 -- -40.33 -50.00 0.00 172 47 \w -108.00 -17.00 0.50 0.20 -- -40.33 -64.00 150.00 182 48 \w -108.00 -17.00 0.50 0.20 -- -40.33 -64.00 90.00 182 49 \w -109.00 -52.00 0.50 0.20 -- -40.33-155.00 -18.00 114 50 \w -146.00 -52.00 0.50 0.20 -- -82.50-155.00 -18.00 188 51 \w -149.00 -75.00 0.50 0.20 -- -82.50-121.00 138.00 148 52 \w -153.00 -78.00 0.50 0.20 -- -82.50 -87.00 30.00 150 53 \w -156.00 -58.00 0.50 0.20 -- -82.50 -17.00-120.00 196 54 \w -83.00 -14.00 0.50 0.20 -- -82.50 68.00 60.00 138 55 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 90.00 64 56 \w -107.00 -27.00 0.50 0.20 -- -40.33 155.00 19.00 160 57 \w -85.00 -9.00 0.50 0.20 -- -40.33 121.00-138.00 152 58 \w -84.00 -15.00 0.50 0.20 -- -82.50 121.00-138.00 138 59 \w -47.00 -15.00 0.50 0.20 -- -82.50 42.00 -90.00 64 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0201922000 _diffrn_orient_matrix_UB_12 -0.0255323000 _diffrn_orient_matrix_UB_13 0.1025627000 _diffrn_orient_matrix_UB_21 0.2833392000 _diffrn_orient_matrix_UB_22 0.0338606000 _diffrn_orient_matrix_UB_23 0.0003083000 _diffrn_orient_matrix_UB_31 -0.1196839000 _diffrn_orient_matrix_UB_32 0.1005275000 _diffrn_orient_matrix_UB_33 0.0120087000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16451 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.182 _diffrn_reflns_theta_min 2.962 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.905 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.33070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellowish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.522 _exptl_crystal_description block _exptl_crystal_F_000 500 _exptl_crystal_preparation 'crystallisation done in chloroform' _exptl_crystal_recrystallization_method 'kept in the chloroform solution' _exptl_crystal_size_max 0.002 _exptl_crystal_size_mid 0.001 _exptl_crystal_size_min 0.001 _refine_diff_density_max 0.583 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef 0.0026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 292 _refine_ls_number_reflns 3872 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0394 _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^)+(0.0686P)^2^+0.5955P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1069 _refine_ls_wR_factor_ref 0.1079 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3682 _reflns_number_total 3872 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cc04720f2.cif _cod_data_source_block ksk_kc_65_auto _cod_database_code 1572880 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H N O Br' _chemical_oxdiff_usercomment 100K _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 0.997 _shelx_estimated_absorpt_t_min 0.994 _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: C2(H2), C1(H1) 2.b Aromatic/amide H refined with riding coordinates: C19(H19), C27(H27), C18(H18), C6(H6), C28(H28), C31(H31), C16(H16), C15(H15), C30(H30), C9(H9), C7(H7), C8(H8) 2.c Idealised Me refined as rotating group: C22(H22A,H22B,H22C), C21(H21A,H21B,H21C) ; _shelx_res_file ; TITL ksk_kc_65_auto.res created by SHELXL-2018/3 at 02:48:56 on 15-Apr-2023 CELL 1.54184 5.039905 14.266752 15.136989 82.4456 83.3581 85.9012 ZERR 2 0.000077 0.000155 0.000206 0.001 0.0012 0.0011 LATT 1 SFAC C H Br N O UNIT 52 40 2 2 8 L.S. 4 PLAN 5 SIZE 0.001 0.001 0.002 TEMP -173.15(10) CONF MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.068600 0.595500 EXTI 0.002622 FVAR 5.64542 BR32 3 0.278929 0.380141 0.151192 11.00000 0.02951 0.05663 = 0.03031 -0.02493 0.00169 0.00920 O3 5 1.584571 0.148550 -0.158636 11.00000 0.01807 0.01811 = 0.01429 -0.00464 -0.00163 -0.00088 O11 5 1.427960 0.073223 -0.397542 11.00000 0.02621 0.01704 = 0.01592 -0.00436 -0.00510 0.00062 O25 5 1.095202 0.184093 -0.404272 11.00000 0.02608 0.01892 = 0.01943 -0.00051 -0.00640 -0.00205 O24 5 1.174469 0.075375 -0.057775 11.00000 0.02895 0.01634 = 0.02977 -0.00018 0.00544 -0.00125 C19 1 1.182240 0.428036 -0.255934 11.00000 0.01916 0.02112 = 0.02184 -0.00372 0.00186 0.00141 AFIX 43 H19 2 1.017420 0.425057 -0.218517 11.00000 -1.20000 AFIX 0 N20 4 1.611542 0.610160 -0.384894 11.00000 0.03503 0.01345 = 0.03113 0.00296 -0.00484 -0.00301 C27 1 0.752121 0.167285 0.039845 11.00000 0.02295 0.02376 = 0.01580 0.00092 -0.00324 0.00009 AFIX 43 H27 2 0.758589 0.100082 0.045267 11.00000 -1.20000 AFIX 0 C5 1 1.686731 0.038853 -0.270069 11.00000 0.01808 0.01409 = 0.01623 -0.00059 0.00053 -0.00375 C18 1 1.269692 0.515834 -0.293414 11.00000 0.02943 0.01590 = 0.02579 -0.00496 -0.00226 0.00449 AFIX 43 H18 2 1.164423 0.571580 -0.281393 11.00000 -1.20000 AFIX 0 C6 1 1.889158 -0.017254 -0.228548 11.00000 0.02156 0.01679 = 0.01882 -0.00121 -0.00179 -0.00248 AFIX 43 H6 2 1.932159 -0.006182 -0.171470 11.00000 -1.20000 AFIX 0 C14 1 1.328218 0.343908 -0.271334 11.00000 0.01949 0.01605 = 0.01480 -0.00259 -0.00333 -0.00048 C28 1 0.552362 0.215231 0.089345 11.00000 0.02234 0.03879 = 0.01388 -0.00045 -0.00049 -0.00187 AFIX 43 H28 2 0.422502 0.181424 0.129220 11.00000 -1.20000 AFIX 0 C26 1 0.945259 0.216890 -0.018282 11.00000 0.02035 0.02114 = 0.01297 -0.00348 -0.00178 0.00007 C13 1 1.337220 0.166854 -0.276656 11.00000 0.01832 0.01282 = 0.01593 -0.00154 -0.00011 -0.00364 C10 1 1.625539 0.021473 -0.354096 11.00000 0.02048 0.01443 = 0.01912 -0.00174 -0.00081 -0.00329 C31 1 0.930461 0.316071 -0.027274 11.00000 0.02435 0.02153 = 0.02079 -0.00532 -0.00048 -0.00313 AFIX 43 H31 2 1.059353 0.350267 -0.067221 11.00000 -1.20000 AFIX 0 C2 1 1.361501 0.214756 -0.136663 11.00000 0.01881 0.01536 = 0.01387 -0.00388 -0.00096 -0.00007 AFIX 13 H2 2 1.424586 0.269627 -0.111562 11.00000 -1.20000 AFIX 0 C17 1 1.512286 0.523255 -0.348973 11.00000 0.02785 0.01503 = 0.02046 0.00050 -0.00668 -0.00347 C29 1 0.543521 0.313837 0.080109 11.00000 0.02251 0.03863 = 0.01651 -0.01294 -0.00250 0.00390 C16 1 1.655416 0.438399 -0.365959 11.00000 0.02123 0.01838 = 0.02199 0.00046 0.00071 -0.00249 AFIX 43 H16 2 1.817508 0.440895 -0.404843 11.00000 -1.20000 AFIX 0 C15 1 1.567021 0.351099 -0.327626 11.00000 0.01971 0.01744 = 0.01788 -0.00192 -0.00075 0.00050 AFIX 43 H15 2 1.670870 0.295143 -0.339894 11.00000 -1.20000 AFIX 0 C30 1 0.729495 0.364516 0.021607 11.00000 0.02699 0.02512 = 0.02793 -0.01097 -0.00496 0.00160 AFIX 43 H30 2 0.718983 0.431779 0.015174 11.00000 -1.20000 AFIX 0 C9 1 1.763738 -0.049721 -0.398079 11.00000 0.02997 0.02172 = 0.02137 -0.00909 -0.00178 -0.00146 AFIX 43 H9 2 1.721979 -0.061045 -0.455229 11.00000 -1.20000 AFIX 0 C1 1 1.234352 0.249120 -0.226260 11.00000 0.01648 0.01595 = 0.01466 -0.00272 -0.00002 -0.00181 AFIX 13 H1 2 1.034625 0.251253 -0.215313 11.00000 -1.20000 AFIX 0 C22 1 1.809271 0.612840 -0.462782 11.00000 0.03946 0.02414 = 0.02637 0.00767 -0.00575 -0.01138 AFIX 137 H22A 2 1.973302 0.576971 -0.446399 11.00000 -1.50000 H22B 2 1.849088 0.678707 -0.484231 11.00000 -1.50000 H22C 2 1.738937 0.584653 -0.510311 11.00000 -1.50000 AFIX 0 C7 1 2.025128 -0.088918 -0.271983 11.00000 0.02403 0.02046 = 0.02853 -0.00298 -0.00419 0.00220 AFIX 43 H7 2 2.160257 -0.128014 -0.244166 11.00000 -1.20000 AFIX 0 C8 1 1.964182 -0.103822 -0.356419 11.00000 0.03032 0.01989 = 0.03020 -0.01050 0.00085 0.00336 AFIX 43 H8 2 2.062261 -0.152152 -0.386068 11.00000 -1.20000 AFIX 0 C21 1 1.440131 0.695522 -0.377258 11.00000 0.04114 0.01321 = 0.05421 -0.00032 -0.01335 -0.00052 AFIX 137 H21A 2 1.287267 0.694151 -0.411534 11.00000 -1.50000 H21B 2 1.541790 0.751080 -0.400986 11.00000 -1.50000 H21C 2 1.375590 0.698976 -0.314099 11.00000 -1.50000 AFIX 0 C12 1 1.269432 0.146234 -0.361049 11.00000 0.02014 0.01262 = 0.01712 -0.00094 0.00029 -0.00333 C4 1 1.535196 0.117139 -0.235478 11.00000 0.01677 0.01501 = 0.01336 -0.00150 0.00265 -0.00636 C23 1 1.161221 0.161310 -0.068381 11.00000 0.02132 0.01817 = 0.01599 -0.00114 -0.00228 -0.00320 HKLF 4 REM REM wR2 = 0.1079, GooF = S = 1.049, Restrained GooF = 1.049 for all data REM R1 = 0.0394 for 3682 Fo > 4sig(Fo) and 0.0404 for all 3872 data REM 292 parameters refined using 0 restraints END WGHT 0.0686 0.5955 REM Highest difference peak 0.583, deepest hole -0.834, 1-sigma level 0.075 Q1 1 0.4413 0.3378 0.1422 11.00000 0.05 0.58 Q2 1 0.1145 0.4214 0.1572 11.00000 0.05 0.52 Q3 1 0.1775 0.4797 0.1740 11.00000 0.05 0.47 Q4 1 0.3826 0.4384 0.1185 11.00000 0.05 0.46 Q5 1 0.4133 0.4166 0.1811 11.00000 0.05 0.46 ; _shelx_res_checksum 11369 _shelx_hkl_file ; 0 0 1 23689.8 579.071 43 0 0 1 25012.3 571.718 47 0 0 -1 23075.0 572.441 1 0 0 -1 23643.1 580.049 11 0 0 2 52398.9 1324.63 45 0 0 2 58458.2 1328.06 43 0 0 2 50052.8 1301.21 47 0 0 -2 55073.3 1350.05 46 0 0 -2 58140.7 1329.39 11 0 0 -2 56609.1 1313.06 1 0 0 3 82844.7 1801.89 45 0 0 3 74092.3 1784.36 43 0 0 -3 78650.2 1835.43 46 0 0 3 69999.5 1753.54 47 0 0 -3 68108.0 1758.70 1 0 0 -3 70585.3 1782.46 11 0 0 4 116059. 2841.60 43 0 0 -4 117973. 2905.17 46 0 0 4 120652. 2815.73 47 0 0 -4 116924. 2854.58 11 0 0 5 38371.7 1071.07 43 0 0 -5 36649.9 1127.05 46 0 0 5 35129.8 1025.75 47 0 0 -5 37085.3 1076.37 11 0 0 5 39112.2 1066.56 3 0 0 5 37381.6 1173.46 10 0 0 6 441.934 78.9518 43 0 0 -6 394.718 82.4288 42 0 0 -6 652.956 109.428 46 0 0 -6 410.001 78.8466 11 0 0 6 624.014 90.8702 3 0 0 6 346.076 89.3591 10 0 0 7 20430.4 752.087 43 0 0 -7 24409.6 853.921 42 0 0 -7 21399.2 843.849 46 0 0 -7 20926.1 778.740 11 0 0 7 25614.1 935.187 10 0 0 7 22210.4 756.358 3 0 0 8 71976.6 2071.21 43 0 0 -8 75237.6 2210.50 46 0 0 8 69633.2 2048.49 3 0 0 8 74376.6 2267.87 10 0 0 -9 117763. 3121.89 42 0 0 -9 124300. 3109.90 11 0 0 9 113095. 3216.02 10 0 0 9 115638. 3002.75 3 0 0 -9 115158. 3162.82 46 0 0 -10 96947.2 2632.82 46 0 0 -10 91691.5 2716.91 52 0 0 -10 89687.8 2544.25 42 0 0 10 82892.3 2379.45 3 0 0 10 90492.2 2639.19 10 0 0 -10 84686.0 2466.34 11 0 0 -10 82732.5 2347.55 16 0 0 10 83615.9 2581.05 14 0 0 -11 3296.96 367.654 46 0 0 -11 3616.27 410.849 52 0 0 -11 4183.96 408.372 42 0 0 11 2829.14 325.293 2 0 0 -11 3218.53 338.100 11 0 0 11 3070.43 298.952 3 0 0 11 3117.39 369.823 10 0 0 -11 2938.38 289.732 16 0 0 11 3620.49 389.661 14 0 0 -12 2895.39 363.859 46 0 0 -12 3554.74 424.050 52 0 0 12 3426.27 368.734 2 0 0 12 2567.65 290.922 3 0 0 -12 3330.20 386.944 42 0 0 12 2913.46 366.642 14 0 0 -12 2794.56 292.258 16 0 0 13 33699.8 1383.56 14 0 0 -13 32992.4 1444.03 52 0 0 14 11990.5 787.372 14 0 0 -14 11074.9 646.316 16 0 0 -14 13232.8 876.204 52 0 0 -15 163.453 109.208 52 0 0 15 223.018 114.479 14 0 0 -15 291.371 100.297 16 0 0 16 38405.7 1489.98 14 0 0 -16 39711.4 1573.41 52 0 0 17 6588.96 471.713 14 0 0 -17 6075.30 479.502 52 0 -1 17 4808.65 391.038 14 0 1 -17 4367.02 331.689 16 0 1 -16 1050.60 175.442 16 0 -1 16 1548.85 248.598 14 0 1 -16 1361.86 247.261 52 0 1 -15 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5170.23 532.646 34 1 9 12 18134.9 954.666 54 1 9 12 16991.6 1013.19 34 1 9 13 13963.5 815.747 54 -1 -9 -13 14571.0 900.420 17 1 9 13 14517.6 892.574 34 1 9 14 1920.54 277.921 54 1 9 14 1871.93 295.501 34 -1 -9 -14 1954.68 307.667 17 1 9 15 8847.18 603.634 34 -1 -9 -15 10640.4 687.411 17 1 9 16 9449.30 560.643 34 -1 -9 -16 11339.1 653.530 17 1 10 -12 10.5881 41.6360 30 -1 -10 12 45.5565 70.8098 14 1 10 -12 22.7906 40.9060 39 1 10 -11 960.956 194.929 52 1 10 -11 1415.82 236.625 30 1 10 -11 1276.67 231.796 39 -1 -10 11 1149.81 223.685 14 1 10 -10 2201.36 332.530 39 -1 -10 10 2695.37 362.331 14 1 10 -10 2281.27 319.109 52 1 10 -9 147.594 98.2891 39 1 10 -9 207.771 94.1574 21 -1 -10 9 184.520 114.774 14 1 10 -9 105.416 84.6840 52 1 10 -8 4357.64 486.180 39 1 10 -8 3045.86 401.387 52 1 10 -8 3592.00 370.324 21 1 10 -7 8534.38 689.713 52 1 10 -7 9644.49 623.961 21 1 10 -6 15583.3 957.937 52 1 10 -6 17960.0 891.489 21 1 10 -5 103.707 75.2139 31 1 10 -5 17.2414 47.9490 52 -1 -10 5 38.5994 53.6709 48 1 10 -5 64.8523 69.0634 21 -1 -10 4 10593.0 783.740 48 1 10 -4 11347.5 756.795 52 1 10 -4 13883.3 796.587 31 -1 -10 4 12109.2 839.953 10 1 10 -4 12065.3 691.520 21 -1 -10 3 2007.70 318.697 48 1 10 -3 2416.10 321.066 31 -1 -10 3 1979.49 330.366 10 1 10 -3 1960.50 255.571 21 -1 -10 2 118.580 81.6562 48 1 10 -2 203.564 93.6582 50 1 10 -2 172.343 77.4083 21 1 10 -2 266.549 118.909 31 -1 -10 2 55.0273 83.3565 10 -1 -10 2 201.282 104.344 8 -1 -10 1 17235.3 987.165 10 -1 -10 1 15802.3 905.060 8 -1 -10 1 14180.8 842.438 7 1 10 -1 15784.3 804.958 56 1 10 -1 17590.6 859.644 50 -1 -10 1 15115.3 889.370 48 1 10 -1 17604.2 873.189 22 1 10 -1 14739.5 778.178 41 1 10 -1 17696.4 880.882 32 1 10 -1 18759.3 949.972 31 -1 -10 0 78502.7 2481.40 10 -1 -10 0 72356.4 2308.77 7 1 10 0 62546.7 2124.61 56 -1 -10 0 62857.9 2225.52 48 1 10 0 70963.8 2218.29 50 1 10 0 65128.6 2133.06 49 1 10 0 73545.1 2247.55 22 1 10 0 62975.8 2107.07 41 1 10 0 76662.5 2284.60 32 1 10 0 62265.1 2025.82 24 1 10 0 68310.9 2231.49 29 1 10 0 83198.0 2365.12 31 -1 -10 -1 10059.7 721.459 10 -1 -10 -1 9591.18 658.069 7 1 10 1 10034.7 614.823 56 -1 -10 -1 9306.80 641.279 48 1 10 1 9755.70 625.047 50 1 10 1 8994.31 578.672 49 1 10 1 11694.5 688.393 22 1 10 1 9704.03 600.517 41 1 10 1 11486.2 688.698 32 1 10 1 12149.7 712.886 31 1 10 1 8809.17 611.013 29 1 10 1 8584.77 612.841 28 1 10 1 9526.78 556.659 24 -1 -10 -2 3584.15 393.751 7 1 10 2 4305.99 384.328 56 1 10 2 3902.80 385.492 50 1 10 2 4132.35 376.942 49 1 10 2 4221.50 400.469 22 1 10 2 4127.14 374.824 41 1 10 2 2977.21 319.223 38 1 10 2 4553.91 419.325 32 1 10 2 3873.92 345.470 24 1 10 2 4562.81 418.299 31 1 10 2 3598.91 380.917 28 1 10 2 3806.43 385.172 29 -1 -10 -3 1773.39 276.847 7 1 10 3 1535.52 227.283 56 1 10 3 2048.06 275.719 50 1 10 3 1890.03 252.114 49 1 10 3 1521.15 217.607 23 1 10 3 1808.32 256.994 22 1 10 3 1283.14 211.256 38 1 10 3 1509.58 227.451 41 1 10 3 2102.52 285.052 32 1 10 3 1501.99 244.264 29 1 10 3 1472.57 213.568 24 1 10 3 1110.11 215.773 28 -1 -10 -4 9310.51 665.987 7 1 10 4 9138.49 571.007 56 1 10 4 9190.96 585.554 50 1 10 4 9300.72 596.681 22 1 10 4 9172.65 560.023 23 1 10 4 7045.92 526.346 38 1 10 4 8364.17 545.135 41 1 10 4 10558.5 651.886 32 1 10 4 8699.21 609.058 29 1 10 4 9573.01 552.779 24 1 10 4 8219.78 599.410 28 1 10 5 6790.87 545.520 29 1 10 5 8081.43 504.151 24 1 10 5 6280.27 539.219 28 -1 -10 -5 9659.97 685.292 46 1 10 5 8105.72 535.501 50 1 10 5 7647.29 527.670 22 1 10 5 8044.54 523.891 23 1 10 5 5549.44 470.242 38 1 10 5 7311.12 496.697 41 1 10 5 8382.56 562.012 32 1 10 5 5595.37 472.281 2 -1 -10 -6 7208.55 613.195 46 1 10 6 5644.99 449.035 23 1 10 6 4210.37 409.064 38 1 10 6 6103.91 429.157 24 1 10 6 5451.49 497.049 28 1 10 6 4898.21 471.657 29 1 10 6 4331.47 422.121 2 -1 -10 -6 5373.97 514.767 9 1 10 7 8477.42 629.512 2 -1 -10 -7 9723.72 732.494 9 1 10 7 12851.6 746.644 54 -1 -10 -7 14377.2 905.826 46 1 10 7 10986.2 644.841 23 1 10 7 7807.81 578.729 38 1 10 7 10387.3 714.425 34 1 10 7 9616.15 684.997 29 1 10 7 9229.26 683.918 28 1 10 8 2419.46 341.237 2 -1 -10 -8 3173.22 421.278 9 1 10 8 3850.71 409.837 54 -1 -10 -8 4096.53 495.596 46 1 10 8 2725.89 327.903 38 1 10 8 3885.91 437.108 34 1 10 8 3144.38 395.388 29 1 10 8 3081.02 388.737 28 1 10 8 3542.77 355.456 23 1 10 9 79221.0 2651.41 34 1 10 9 71456.5 2539.03 28 1 10 9 77419.3 2601.17 29 1 10 9 72582.8 2352.98 23 1 10 10 29551.6 1203.72 55 1 10 10 32115.3 1348.62 54 1 10 10 30477.0 1397.13 34 1 10 10 26970.2 1291.57 28 1 10 10 28629.9 1177.76 23 1 10 11 9638.01 669.857 54 1 10 11 8905.93 582.388 55 1 10 11 7860.51 615.721 28 1 10 11 8088.17 676.130 34 1 10 12 15739.1 889.715 54 1 10 12 15189.0 921.614 34 1 10 13 27903.2 1231.17 54 1 10 13 27309.9 1257.76 34 1 10 14 2170.25 285.840 54 1 10 14 2051.00 289.914 34 1 10 15 1011.45 184.516 34 1 10 16 3758.23 304.623 34 1 11 -11 144.129 75.5783 30 1 11 -10 6047.76 489.835 30 1 11 -10 3947.42 335.748 21 1 11 -9 348.343 132.157 30 1 11 -9 157.027 80.6595 21 1 11 -8 15408.7 800.650 21 1 11 -7 4414.19 414.129 21 1 11 -6 38545.9 1470.04 21 1 11 -5 6121.47 531.634 31 1 11 -5 5001.62 447.218 21 1 11 -4 1436.25 261.734 31 1 11 -4 1048.49 199.402 21 -1 -11 3 1234.55 271.274 48 1 11 -3 963.260 187.401 21 -1 -11 2 969.895 235.905 48 1 11 -2 851.870 187.239 50 1 11 -2 620.616 149.685 21 1 11 -2 1142.71 233.735 31 -1 -11 2 1177.86 270.818 10 -1 -11 1 8431.38 710.838 10 -1 -11 1 7030.99 626.225 8 1 11 -1 6558.80 517.595 56 -1 -11 1 7122.07 620.145 48 1 11 -1 6801.08 534.394 50 1 11 -1 6825.09 539.696 22 1 11 -1 6308.11 500.356 41 1 11 -1 7176.12 553.496 32 1 11 -1 7372.74 600.228 31 -1 -11 0 3452.17 454.786 10 -1 -11 0 2747.64 372.328 7 1 11 0 2500.11 316.791 56 -1 -11 0 2288.24 341.328 48 1 11 0 3180.80 362.275 50 1 11 0 3390.18 381.419 22 1 11 0 2712.63 325.945 41 1 11 0 3744.66 402.635 32 1 11 0 2995.92 314.353 24 -1 -11 -1 1045.45 267.389 10 -1 -11 -1 821.854 207.534 7 1 11 1 693.806 167.876 56 1 11 1 1194.56 227.516 50 1 11 1 1305.69 235.161 22 1 11 1 766.631 177.285 41 1 11 1 1051.81 220.435 32 1 11 1 882.777 205.080 29 1 11 1 919.952 205.267 31 -1 -11 -2 32287.8 1469.68 10 -1 -11 -2 23158.2 1199.61 7 1 11 2 23868.2 1086.31 56 1 11 2 26522.5 1151.81 50 1 11 2 24477.6 1136.80 22 1 11 2 24249.9 1100.52 41 1 11 2 27553.3 1201.46 32 1 11 2 24015.2 1032.88 24 1 11 2 22758.8 1110.67 29 1 11 2 29875.7 1217.45 31 1 11 2 21669.8 1110.89 28 -1 -11 -3 56368.6 2093.65 7 1 11 3 55602.4 1884.05 56 1 11 3 61507.2 1970.82 50 1 11 3 62606.0 1989.34 22 1 11 3 56576.2 1836.96 23 1 11 3 56111.2 1895.79 41 1 11 3 45623.6 1797.47 38 1 11 3 64599.6 2029.51 32 1 11 3 54280.7 1944.75 29 1 11 3 55677.5 1833.98 24 1 11 3 52039.3 1955.88 28 -1 -11 -4 19878.4 1091.20 7 1 11 4 17729.8 886.266 56 1 11 4 20268.5 948.830 50 1 11 4 17109.3 849.236 23 1 11 4 18969.6 932.518 22 1 11 4 17388.0 874.825 41 1 11 4 19412.6 948.034 32 1 11 4 17885.6 944.049 29 1 11 4 16567.6 940.064 28 1 11 4 17511.6 848.432 24 1 11 5 834.739 168.752 24 1 11 5 461.871 148.539 29 1 11 5 321.679 130.630 28 1 11 5 520.803 150.308 50 1 11 5 171.737 95.1200 38 1 11 5 331.561 112.460 41 -1 -11 -5 321.797 144.647 7 1 11 5 357.564 127.116 32 1 11 5 574.743 154.966 22 1 11 5 429.771 133.341 23 1 11 6 31319.8 1409.12 38 1 11 6 36578.3 1573.43 28 1 11 6 39464.1 1397.87 24 1 11 6 41152.8 1593.97 29 1 11 6 40905.9 1478.57 23 -1 -11 -6 48602.9 1882.30 7 1 11 7 24616.7 1086.50 23 1 11 7 24015.5 1197.95 28 1 11 7 24989.5 1175.97 29 1 11 8 14934.6 893.974 34 1 11 8 13875.9 849.689 29 1 11 8 13989.2 883.934 28 1 11 8 15224.3 798.736 23 1 11 9 4976.15 465.988 54 1 11 9 4631.31 485.620 34 1 11 9 4224.90 468.504 28 1 11 9 4678.39 419.311 23 1 11 10 7386.34 584.960 54 1 11 10 6617.36 585.633 34 1 11 10 5761.20 541.862 28 1 11 10 6489.23 492.364 23 1 11 11 41963.7 1693.32 34 1 11 11 38268.8 1608.40 28 1 11 11 41948.6 1493.93 23 1 11 12 2586.18 336.495 54 1 11 12 1945.94 282.051 28 1 11 12 2375.31 331.677 34 1 11 13 84.8951 75.4004 34 1 11 13 279.766 116.724 54 1 11 14 891.949 177.515 34 1 11 14 1456.21 223.222 54 1 11 15 1448.17 196.169 34 1 12 -10 659.518 146.877 30 1 12 -10 569.944 112.469 21 1 12 -9 91.5834 72.7647 30 1 12 -9 38.2956 48.6158 21 1 12 -8 11951.5 733.849 30 1 12 -8 9286.95 575.007 21 1 12 -7 3707.49 411.100 30 1 12 -7 2725.19 315.542 21 1 12 -6 6834.20 577.873 30 1 12 -6 4772.66 441.478 21 1 12 -5 1062.01 225.997 31 1 12 -5 1056.57 206.532 21 1 12 -4 82.8400 84.1099 31 1 12 -4 27.0675 53.2248 21 1 12 -3 84.7278 86.0325 31 1 12 -3 52.8112 56.0919 21 1 12 -2 4165.08 418.973 50 1 12 -2 4705.77 484.839 31 1 12 -2 4022.16 382.728 21 1 12 -1 4251.61 432.265 50 1 12 -1 3905.09 417.607 32 1 12 -1 4672.62 477.252 31 1 12 -1 3523.29 393.617 22 1 12 0 24737.0 1141.87 50 1 12 0 24046.6 1144.59 32 1 12 0 27268.2 1223.83 31 1 12 0 20030.6 965.085 24 1 12 0 22967.0 1106.53 22 1 12 1 11034.7 723.331 50 1 12 1 11855.2 766.477 32 1 12 1 9891.07 631.653 24 1 12 1 10963.0 727.542 22 1 12 2 13022.3 783.557 50 1 12 2 14222.3 833.187 32 1 12 2 11745.8 693.944 24 1 12 2 13474.4 808.418 31 1 12 2 10981.6 762.741 28 1 12 2 12825.6 797.719 29 1 12 2 12404.0 775.143 22 1 12 3 121.137 87.6432 50 1 12 3 45.5322 73.0944 22 1 12 3 62.3314 79.1061 32 1 12 3 17.0811 67.1676 28 1 12 3-12.7007 61.1675 24 1 12 3 15.8659 62.3896 29 1 12 4 56793.6 1870.16 50 1 12 4 46384.9 1704.52 23 1 12 4 55348.4 1862.60 22 1 12 4 41626.6 1712.01 38 1 12 4 58334.0 1908.68 32 1 12 4 52143.4 1881.72 29 1 12 4 47078.0 1693.78 24 1 12 4 48742.2 1886.66 28 1 12 5 1095.41 218.998 50 1 12 5 714.594 185.121 38 1 12 5 769.725 179.637 23 1 12 5 807.251 184.148 22 1 12 5 818.110 191.347 32 1 12 5 909.140 213.421 29 1 12 5 609.223 155.615 24 1 12 5 743.590 210.692 28 1 12 6 3161.45 374.795 38 1 12 6 4154.31 401.864 23 1 12 6 3205.43 336.272 24 1 12 6 3889.82 426.843 29 1 12 6 3573.41 429.870 28 1 12 7 2157.61 312.058 38 1 12 7 3487.53 369.998 23 1 12 7 3383.40 334.373 24 1 12 7 3486.96 426.849 28 1 12 8 64550.6 2068.26 23 1 12 8 66748.3 2234.20 34 1 12 8 66408.7 2293.74 28 1 12 9 269.630 112.922 54 1 12 9 161.122 91.6115 38 1 12 9 135.081 101.569 34 1 12 9 309.244 137.077 28 1 12 10 32235.5 1326.58 54 1 12 10 28276.3 1301.36 34 1 12 10 28021.3 1315.77 28 1 12 10 29572.9 1192.23 23 1 12 11 8608.23 618.190 54 1 12 11 7862.03 598.920 34 1 12 11 6865.45 559.358 28 1 12 11 7148.07 495.674 23 1 12 12 26313.5 1120.99 54 1 12 12 24696.2 1101.33 34 1 12 13 2615.25 301.353 34 1 12 13 2988.99 323.331 54 1 12 14 1500.12 203.647 34 1 13 -9 2654.92 244.710 21 1 13 -9 3367.99 311.188 30 1 13 -8 65.6303 54.2908 21 1 13 -8 82.4066 62.6987 30 1 13 -7 1235.38 196.788 21 1 13 -7 1453.67 235.271 30 1 13 -6 1962.13 259.452 21 1 13 -5 5047.50 432.502 21 1 13 -5 5133.88 474.879 31 1 13 -4 105.341 73.2817 21 1 13 -4 175.705 99.3520 31 1 13 -3 2079.05 281.810 21 1 13 -3 2609.02 349.610 31 1 13 -2 3740.91 376.119 21 1 13 -2 5792.18 538.527 31 1 13 -1 6517.45 536.911 22 1 13 -1 6502.72 544.433 50 1 13 -1 7530.32 587.826 32 1 13 -1 7744.78 626.591 31 1 13 0 1058.08 220.572 22 1 13 0 1072.53 222.108 50 1 13 0 1111.42 230.716 32 1 13 0 1014.20 228.365 31 1 13 0 1191.77 207.617 24 1 13 1 268.787 132.082 22 1 13 1 624.471 174.482 50 1 13 1 388.455 144.845 32 1 13 1 246.253 126.595 31 1 13 1 245.604 115.761 24 1 13 2 10209.2 694.718 22 1 13 2 11560.2 739.023 50 1 13 2 10838.2 729.589 32 1 13 2 10866.5 721.284 31 1 13 3 4759.84 459.865 22 1 13 3 4891.44 469.477 50 1 13 3 4883.49 476.095 32 1 13 3 4892.54 480.228 29 1 13 3 4479.86 480.243 28 1 13 3 4475.91 417.529 24 1 13 4 21835.6 1023.79 23 1 13 4 22576.9 1077.09 22 1 13 4 25238.6 1136.80 50 1 13 4 23585.6 1102.57 32 1 13 4 20421.2 1109.83 28 1 13 4 19389.2 963.390 24 1 13 4 22336.5 1102.34 29 1 13 5 1101.70 215.806 22 1 13 5 1019.07 209.005 23 1 13 5 1378.84 241.774 50 1 13 5 1212.81 227.979 32 1 13 5 1137.79 246.086 28 1 13 5 1115.54 207.160 24 1 13 6 23156.1 1051.49 32 1 13 6 20484.2 952.867 24 1 13 6 21982.8 1148.25 28 1 13 6 21186.0 1009.12 23 1 13 7 18.4998 83.9976 28 1 13 7-11.5199 48.9288 24 1 13 7 109.642 82.3197 23 1 13 8 14118.4 884.673 28 1 13 8 13436.1 757.035 23 1 13 9 6327.01 561.737 28 1 13 9 6818.99 508.866 23 1 13 10 3040.03 355.047 34 1 13 10 3304.62 384.149 28 1 13 10 2800.52 306.765 23 1 13 11 970.506 193.300 54 1 13 11 638.034 159.992 34 1 13 11 591.931 158.622 28 1 13 11 714.535 149.833 23 1 13 12 11.2487 44.2462 34 1 13 12 216.224 89.5036 28 1 13 13 2328.34 247.977 34 1 13 13 2438.29 250.147 28 1 14 -8 13.8052 33.2432 21 1 14 -7 644.764 128.065 21 1 14 -6 365.263 105.443 21 1 14 -5 102.635 77.0869 31 1 14 -5 87.0950 60.5765 21 1 14 -4 853.301 194.527 31 1 14 -4 738.032 160.228 21 1 14 -3 371.731 134.155 31 1 14 -3 366.388 117.252 21 1 14 -2 111.771 92.4511 31 1 14 -1 2535.44 329.302 50 1 14 -1 3204.39 365.004 32 1 14 -1 3271.46 389.664 31 1 14 -1 2744.40 329.018 22 1 14 0 6061.11 518.656 50 1 14 0 5584.24 494.435 32 1 14 0 4301.38 390.105 24 1 14 0 6338.28 547.560 31 1 14 0 5238.29 472.215 22 1 14 1 727.371 184.830 50 1 14 1 604.800 173.100 32 1 14 1 691.868 159.345 24 1 14 1 608.336 168.616 31 1 14 1 631.321 167.823 22 1 14 2 6303.72 537.297 50 1 14 2 7212.17 570.553 32 1 14 2 5293.63 452.217 24 1 14 2 6549.72 536.579 22 1 14 3 21802.1 1042.70 50 1 14 3 21505.1 1037.16 32 1 14 3 19791.7 995.080 22 1 14 4 8409.97 610.814 50 1 14 4 8722.51 615.828 32 1 14 4 6551.90 502.849 24 1 14 4 7206.89 554.065 22 1 14 5 1679.56 265.496 50 1 14 5 1438.40 248.403 32 1 14 5 1208.93 249.825 28 1 14 5 1220.52 208.439 24 1 14 5 1327.68 229.079 22 1 14 5 1293.24 224.917 23 1 14 6 5786.44 476.496 32 1 14 6 4949.19 497.368 28 1 14 6 4647.65 397.673 24 1 14 6 5240.37 454.924 23 1 14 6 5384.32 445.009 22 1 14 7 5634.19 523.183 28 1 14 7 4954.63 397.298 24 1 14 7 6229.48 487.995 23 1 14 8 7160.09 585.278 28 1 14 8 7584.06 533.231 23 1 14 9 9664.73 661.548 28 1 14 9 9393.94 581.717 23 1 14 10 767.131 176.003 28 1 14 10 482.941 126.301 23 1 14 11 1619.14 230.741 28 1 14 11 1587.03 203.117 23 1 14 12 3490.61 304.400 28 1 15 -5 406.980 113.306 31 1 15 -5 191.842 74.7761 21 1 15 -4 1469.52 226.020 31 1 15 -4 1198.84 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18157.9 924.158 18 4 11 4 20378.7 971.999 22 4 11 4 21026.6 993.574 32 4 11 4 19123.8 933.495 50 4 11 5 14093.6 770.389 22 4 11 5 15549.9 806.708 32 4 11 5 14233.9 758.145 50 4 11 6 16856.5 837.709 32 4 11 6 20327.5 826.354 24 4 11 6 18329.0 844.878 22 -4 -11 -6 14556.6 852.516 18 4 11 7 1331.10 235.542 54 4 11 7 1754.65 228.736 55 4 11 7 1563.12 202.147 24 -4 -11 -7 1281.94 238.380 18 4 11 8 113.180 81.2660 54 4 11 8 27.7281 49.2321 55 4 11 8 70.4917 61.6742 23 -4 -11 -8 44.5358 63.0682 18 4 11 8 137.249 71.0018 24 4 11 9 1860.16 211.070 23 -4 -11 -9 1473.26 248.526 18 4 11 9 1774.83 191.800 24 4 11 10 406.602 96.2950 23 -4 -11 -10 474.196 138.355 18 4 11 11 14237.4 577.170 23 -4 -12 3 216.569 88.2726 19 -4 -12 2 9756.89 574.645 19 4 12 -2 9298.93 537.213 31 -4 -12 1 1187.25 208.619 19 4 12 -1 905.134 172.184 31 -4 -12 0 5635.68 463.823 19 4 12 0 5288.60 406.148 22 4 12 0 4661.47 404.857 31 4 12 0 5461.83 411.002 32 4 12 0 5406.18 405.348 50 -4 -12 -1 3170.54 360.907 19 4 12 1 3370.82 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315.963 18 5 2 -3 2762.06 319.221 53 5 2 -2 5091.91 427.973 50 -5 -2 2 4764.75 408.809 35 5 2 -2 5688.12 453.148 53 -5 -2 1 17746.7 900.180 58 5 2 -1 15968.2 815.371 53 -5 -2 1 17184.5 864.878 20 -5 -2 1 18640.9 926.857 51 5 2 -1 16787.7 863.644 50 -5 -2 0 2814.76 351.503 58 5 2 0 2669.40 297.745 53 -5 -2 0 2919.64 349.539 20 -5 -2 0 2936.30 361.574 51 5 2 0 2335.17 313.611 50 -5 -2 -1 159.960 108.947 58 5 2 1 108.776 80.0249 53 -5 -2 -1 74.6802 95.9109 20 -5 -2 -1-16.6127 88.4529 51 5 2 1 85.4924 82.4763 50 -5 -2 -2 2037.76 304.940 20 -5 -2 -2 2090.47 324.031 51 5 2 2 2509.89 322.328 50 -5 -2 -2 2048.34 321.231 58 5 2 2 2608.99 279.751 53 -5 -2 -2 2789.67 309.055 17 -5 -2 -3 6226.23 525.522 20 -5 -2 -3 6323.07 563.340 51 5 2 3 4660.81 439.152 50 -5 -2 -3 5954.82 535.806 58 5 2 3 5608.86 414.661 53 -5 -2 -3 6494.39 489.336 17 -5 -2 -4 58.0635 73.7029 20 -5 -2 -4 98.6470 91.4391 51 5 2 4 103.057 80.1053 50 -5 -2 -4 77.4800 78.6774 58 5 2 4 37.9693 50.5610 53 -5 -2 -4 79.7830 70.8116 17 -5 -2 -5 2366.40 313.098 58 5 2 5 2432.56 257.389 53 -5 -2 -5 2383.56 302.001 20 -5 -2 -5 2154.62 288.144 35 -5 -2 -5 2934.66 342.966 17 -5 -2 -5 2681.63 340.276 51 5 2 5 1713.69 245.430 50 -5 -2 -6 725.053 179.887 17 5 2 6 574.918 125.864 53 -5 -2 -7 5495.62 503.891 17 5 2 7 6828.07 418.911 53 -5 -2 -8 431.482 140.363 17 5 2 8 531.805 113.517 53 -5 -2 -8 471.887 103.314 59 -5 -2 -9 5110.71 477.774 17 5 2 9 7948.19 426.581 53 5 2 10 4378.32 292.757 53 -5 -2 -10 3436.02 362.660 17 -5 -2 -10 3971.40 341.051 37 -5 -2 -11 1809.49 203.266 37 -5 -2 -11 1466.44 219.295 17 -5 -3 7 8003.50 438.368 38 -5 -3 7 8410.28 429.068 18 5 3 -6 4203.68 376.616 53 -5 -3 6 8402.70 445.336 18 5 3 -5 154.663 81.0449 53 -5 -3 5 24.3361 48.7547 36 -5 -3 5 122.116 67.1741 18 5 3 -4 8031.23 564.510 53 -5 -3 4 11726.0 599.457 18 5 3 -3 3952.09 384.864 53 -5 -3 3 5336.17 404.918 18 5 3 -2 2606.00 304.737 53 -5 -3 2 3425.57 333.940 18 -5 -3 1 15876.1 866.157 58 5 3 -1 15908.1 805.532 53 -5 -3 1 17919.7 878.913 20 -5 -3 1 19416.9 868.047 18 -5 -3 1 16809.3 887.452 51 5 3 -1 14357.3 790.151 50 -5 -3 0 9644.17 682.954 58 5 3 0 10303.7 611.779 53 -5 -3 0 10391.8 683.379 20 -5 -3 0 11753.5 664.385 18 -5 -3 0 11136.7 735.000 51 5 3 0 9066.64 618.049 50 -5 -3 -1 4811.78 478.864 58 5 3 1 4645.44 389.211 53 -5 -3 -1 4826.24 469.901 20 -5 -3 -1 5557.65 526.704 51 5 3 1 4072.10 407.528 50 -5 -3 -2 2887.91 383.154 58 5 3 2 3242.33 312.874 53 -5 -3 -2 2646.19 351.816 20 -5 -3 -2 3080.25 398.985 51 5 3 2 2556.07 322.029 50 -5 -3 -3 15144.9 911.628 58 5 3 3 16441.5 749.563 53 -5 -3 -3 16274.7 918.545 20 -5 -3 -3 16605.6 968.076 51 5 3 3 13705.0 786.748 50 -5 -3 -4 7610.79 593.549 20 -5 -3 -4 7521.76 619.613 51 5 3 4 7187.67 523.864 50 5 3 4 8523.51 502.530 53 -5 -3 -4 6644.57 576.689 58 -5 -3 -4 6965.33 518.307 17 -5 -3 -5 969.290 198.490 20 -5 -3 -5 1127.03 230.513 51 5 3 5 570.509 143.618 50 5 3 5 838.364 155.136 53 -5 -3 -5 931.883 203.774 58 -5 -3 -5 967.437 196.252 17 5 3 6 6973.72 428.532 53 -5 -3 -6 5371.64 483.258 17 5 3 7 11327.6 550.825 53 -5 -3 -7 8135.75 615.684 17 5 3 8 670.329 127.594 53 -5 -3 -8 619.161 168.599 17 5 3 9 7699.62 413.832 53 -5 -3 -9 4348.99 439.689 17 -5 -3 -10 2780.01 331.675 17 5 3 10 3469.69 293.860 23 5 3 11 1289.96 158.523 23 -5 -3 -11 1332.07 182.366 37 -5 -3 -11 1395.68 216.942 17 -5 -4 7 383.643 87.9138 18 -5 -4 7 337.506 85.3061 38 5 4 -7 364.089 85.0317 21 -5 -4 6 2595.28 235.891 18 5 4 -6 2968.43 251.821 21 -5 -4 5 1263.13 176.561 18 5 4 -5 929.998 176.138 53 -5 -4 4 729.886 145.766 18 5 4 -4 368.941 115.200 53 -5 -4 3 3948.30 343.009 18 5 4 -3 3212.93 331.812 53 -5 -4 2 1623.72 227.359 18 5 4 -2 1521.79 230.192 53 -5 -4 1 798.247 179.834 20 -5 -4 1 1066.84 190.677 18 -5 -4 1 912.744 197.985 58 5 4 -1 956.719 179.357 53 -5 -4 1 879.108 195.013 51 5 4 -1 801.775 173.422 50 -5 -4 0 180.030 99.4942 20 -5 -4 0 192.469 109.415 58 5 4 0 425.361 120.702 53 -5 -4 0 326.776 116.738 18 -5 -4 0 365.118 141.112 51 5 4 0 260.539 106.813 50 -5 -4 -1 14445.4 861.858 20 -5 -4 -1 15623.7 798.142 18 -5 -4 -1 12878.9 848.379 58 5 4 1 13668.7 703.177 53 -5 -4 -1 15412.0 931.669 51 5 4 1 14730.8 797.399 50 -5 -4 -2 17.0933 82.3184 20 5 4 2-10.1258 53.9112 53 -5 -4 -2 19.3505 53.8028 51 5 4 2 54.0241 61.3231 50 -5 -4 -3 1462.33 274.584 20 -5 -4 -3 1046.83 239.027 58 5 4 3 1266.58 189.261 53 -5 -4 -3 1398.48 283.917 51 5 4 3 1516.97 240.492 50 -5 -4 -4 4865.38 488.204 20 5 4 4 5655.71 395.335 53 -5 -4 -4 5683.34 536.516 58 -5 -4 -4 6098.10 569.491 51 5 4 4 5164.32 439.302 50 -5 -4 -5 449.069 147.462 20 -5 -4 -5 434.104 156.649 51 5 4 5 390.628 121.413 50 -5 -4 -5 524.787 160.932 58 5 4 5 581.757 129.354 53 5 4 6 4881.60 357.570 53 -5 -4 -7 152.800 83.6102 17 5 4 7 357.597 97.3016 53 -5 -4 -8 550.988 158.817 17 5 4 8 142.158 63.7124 53 5 4 9 759.215 127.848 53 -5 -4 -9 411.975 132.799 17 5 4 9 521.240 114.270 24 5 4 9 422.374 115.733 23 5 4 10 3156.85 272.058 23 -5 -4 -10 1941.79 268.426 17 5 4 11 3714.90 272.448 23 -5 -4 -11 3243.71 321.399 17 -5 -5 6 5871.60 356.454 18 5 5 -6 7011.86 384.574 21 -5 -5 5 15493.8 679.443 18 5 5 -5 17834.1 713.774 21 5 5 -4 1327.02 204.080 53 -5 -5 4 1735.01 211.999 18 5 5 -3 11.0750 43.5484 53 -5 -5 3 9.74661 44.2540 18 -5 -5 2 19875.1 840.406 18 5 5 -2 14265.8 756.899 53 -5 -5 1 275.783 117.764 20 -5 -5 1 452.717 142.148 58 5 5 -1 500.756 131.119 53 -5 -5 1 411.354 120.101 18 5 5 -1 523.645 138.862 50 -5 -5 0 10648.9 702.395 20 -5 -5 0 11840.2 659.973 18 5 5 0 9386.72 565.659 53 -5 -5 0 10087.0 720.449 51 5 5 0 10846.1 645.485 50 -5 -5 -1 1983.43 311.824 20 -5 -5 -1 2294.66 290.865 18 5 5 1 1565.66 221.096 53 -5 -5 -1 2015.94 331.351 51 5 5 1 1956.15 269.781 50 -5 -5 -2 8440.53 582.631 18 -5 -5 -2 7425.61 624.052 20 5 5 2 7821.22 489.109 53 -5 -5 -2 6960.82 640.628 51 5 5 2 8022.44 560.236 50 -5 -5 -3 546.957 172.672 20 5 5 3 366.239 109.322 53 -5 -5 -3 567.191 154.293 18 -5 -5 -3 645.532 199.958 51 5 5 3 653.673 158.464 50 -5 -5 -4 3314.88 431.877 51 5 5 4 3522.30 353.423 50 5 5 4 3626.43 308.896 53 -5 -5 -4 3869.23 432.664 20 -5 -5 -5 3666.37 430.561 51 5 5 5 4152.57 368.161 50 5 5 5 3815.25 313.610 53 -5 -5 -5 4054.25 421.222 20 5 5 6 20822.8 805.542 53 5 5 6 17939.2 862.774 23 -5 -5 -6 18161.1 897.286 20 5 5 7 5304.14 346.834 53 5 5 7 4608.76 358.166 24 5 5 8 19243.4 800.584 24 5 5 8 16978.1 829.820 23 5 5 9 2174.78 206.666 53 5 5 9 1868.45 201.919 24 5 5 9 2310.35 244.027 23 5 5 10 906.520 145.421 23 -5 -5 -10 477.992 127.225 17 5 5 10 867.004 153.390 15 5 5 11 6439.07 372.241 23 -5 -5 -11 6653.58 447.879 17 -5 -6 6 1558.34 161.445 18 5 6 -6 1870.26 181.988 21 -5 -6 5 1575.06 179.382 18 5 6 -5 2002.67 202.511 21 -5 -6 4 143.753 69.1151 18 5 6 -3 317.690 97.9780 53 -5 -6 3 287.539 95.9245 18 -5 -6 2 701.884 148.772 18 5 6 -2 628.068 135.675 53 5 6 -1 11.7732 56.7045 22 -5 -6 1 38.1285 61.2132 20 5 6 -1 39.1786 49.7289 53 -5 -6 1 53.7460 59.7811 18 5 6 -1 66.3591 68.7671 50 -5 -6 0 10034.6 703.903 51 5 6 0 10402.5 622.702 50 5 6 0 8758.37 527.415 53 -5 -6 0 8892.98 636.786 20 5 6 0 10199.3 636.464 22 -5 -6 0 9924.05 592.196 18 -5 -6 -1 1694.91 304.003 51 5 6 1 1402.77 227.289 50 5 6 1 999.966 171.074 53 5 6 1 1294.46 226.517 22 -5 -6 -1 1375.65 222.108 18 -5 -6 -2 14952.2 980.750 51 5 6 2 17342.7 850.649 50 5 6 2 17352.6 753.758 53 -5 -6 -2 19847.9 918.079 18 5 6 2 14709.9 837.919 22 -5 -6 -3 3458.91 368.235 18 5 6 3 3270.54 356.826 22 5 6 3 3558.37 307.062 53 -5 -6 -3 2638.97 396.756 51 5 6 3 3929.46 374.598 50 5 6 3 3659.63 330.721 24 -5 -6 -4 1125.21 220.789 18 5 6 4 817.644 178.966 22 5 6 4 1059.92 167.813 53 -5 -6 -4 713.372 207.323 51 5 6 4 1061.19 192.664 50 5 6 4 1047.26 182.144 24 -5 -6 -5 12943.4 775.792 20 5 6 5 14060.5 727.212 22 -5 -6 -5 11415.1 737.345 18 5 6 5 14066.3 625.790 53 -5 -6 -5 12008.4 811.488 51 5 6 5 10913.8 637.786 50 5 6 5 12976.5 663.166 24 5 6 6 8012.98 448.623 53 5 6 6 8263.26 504.211 24 -5 -6 -6 7875.24 554.482 20 5 6 7 194.137 71.2755 53 5 6 7 180.386 88.1689 24 5 6 7 178.047 88.5078 23 5 6 8 60.0654 44.2102 53 5 6 8 120.160 70.4569 24 5 6 8 92.1216 66.1590 23 5 6 9 23158.9 859.253 24 5 6 9 24668.0 973.124 15 5 6 10 3800.60 284.923 23 5 6 10 3312.62 289.705 15 5 6 11 159.636 60.8775 23 5 6 11 267.929 78.1128 15 -5 -7 5 676.137 110.305 18 5 7 -5 786.512 117.703 21 -5 -7 4 1394.02 168.967 18 -5 -7 3 6862.02 414.562 18 -5 -7 2 739.129 142.936 18 5 7 -1 6641.10 466.356 22 -5 -7 1 6430.36 433.098 18 5 7 0 8636.86 557.440 22 -5 -7 0 7726.04 503.698 18 -5 -7 0 6937.44 575.656 51 5 7 0 7658.65 512.587 50 5 7 1 7856.45 548.091 22 -5 -7 -1 8091.47 532.200 18 -5 -7 -1 7151.83 622.051 51 5 7 1 8594.43 553.103 50 -5 -7 -2 7388.34 521.300 18 5 7 2 8307.45 564.045 22 5 7 2 7473.28 521.607 50 -5 -7 -3 1009.20 198.527 18 5 7 3 1205.40 215.962 22 5 7 3 1228.79 186.616 24 -5 -7 -3 654.177 203.746 51 5 7 3 1267.73 209.957 50 -5 -7 -4 38.9854 88.5499 51 5 7 4 137.626 80.3002 50 5 7 4 99.9498 57.9588 53 5 7 4 243.388 103.409 22 -5 -7 -4 124.034 88.5378 18 5 7 4 163.651 78.8474 24 5 7 5 5600.18 429.840 22 -5 -7 -5 4626.13 441.553 18 5 7 5 5819.01 361.148 53 -5 -7 -5 4921.09 500.816 51 5 7 5 5067.76 401.440 50 5 7 5 4979.45 378.653 24 5 7 6 14032.2 598.964 53 5 7 6 15150.7 685.960 24 -5 -7 -6 13135.8 729.771 20 5 7 6 14006.9 689.096 22 5 7 7 13068.7 571.609 53 5 7 7 13288.0 634.346 24 5 7 8 11938.4 627.760 15 5 7 8 12506.8 582.336 24 5 7 9 290.645 84.8833 23 5 7 9 336.827 99.2577 15 5 7 9 310.788 80.1321 24 5 7 10 4172.51 310.319 15 5 7 10 4256.57 290.579 23 -5 -8 4 90.2172 47.0769 18 -5 -8 3 4497.34 308.651 18 -5 -8 2 77.0122 56.6790 18 -5 -8 1 1083.28 170.239 18 5 8 0 8160.58 516.971 22 -5 -8 0 6938.28 454.179 18 -5 -8 0 6437.05 530.068 51 5 8 0 7002.90 470.723 50 5 8 1 7499.03 514.188 22 -5 -8 -1 6746.17 458.493 18 -5 -8 -1 5810.69 538.258 51 5 8 1 7075.97 485.009 50 -5 -8 -2 5287.68 420.032 18 5 8 2 5212.01 424.057 22 -5 -8 -2 3830.58 459.471 51 5 8 2 5188.49 414.816 50 -5 -8 -3 994.176 186.846 18 5 8 3 600.735 148.555 22 -5 -8 -3 498.389 174.810 51 5 8 3 818.079 164.681 50 -5 -8 -4 1010.08 196.606 18 5 8 4 905.188 178.301 22 -5 -8 -4 696.031 193.972 51 5 8 4 925.680 174.084 50 5 8 4 1112.99 170.559 24 5 8 5 6935.03 475.463 22 -5 -8 -5 6325.92 500.823 18 -5 -8 -5 6509.07 560.397 51 5 8 5 7061.41 466.447 50 5 8 6 1845.65 215.242 24 -5 -8 -6 1845.33 243.584 20 5 8 6 1330.43 194.100 22 -5 -8 -6 1492.47 243.527 18 5 8 7 2943.73 258.558 24 -5 -8 -7 2195.99 287.580 18 5 8 8 2633.40 231.979 24 5 8 8 2782.65 247.756 23 5 8 9 66.1415 41.5487 24 5 8 9 137.368 61.2613 23 -5 -9 2 4390.44 296.749 18 -5 -9 1 3033.23 260.300 18 5 9 0 611.237 133.721 32 5 9 0 585.697 129.156 22 -5 -9 0 678.996 130.769 18 5 9 1 1838.36 236.646 32 5 9 1 1773.08 230.263 22 -5 -9 -1 1491.13 198.375 18 5 9 2 179.381 81.3045 22 -5 -9 -2 129.761 86.4233 51 5 9 2 111.730 72.9971 50 5 9 2 160.909 89.5426 32 -5 -9 -2 173.094 77.2583 18 5 9 3 485.499 130.640 22 -5 -9 -3 339.982 136.919 51 5 9 3 659.633 142.478 50 5 9 3 465.000 126.895 32 -5 -9 -3 602.017 138.877 18 -5 -9 -4 2277.62 270.833 18 5 9 4 2537.13 275.269 22 -5 -9 -4 1945.53 303.639 51 5 9 4 2022.87 252.292 32 5 9 4 2791.12 252.121 24 5 9 5 10957.1 601.370 32 5 9 5 11862.8 609.333 22 -5 -9 -5 10660.4 631.508 18 5 9 6 1087.96 154.408 24 5 9 6 862.816 151.111 32 -5 -9 -6 807.739 166.230 18 5 9 6 754.134 138.791 22 5 9 7 10397.0 481.717 24 -5 -9 -7 7464.87 512.478 18 5 9 8 92.3830 49.0942 24 -5 -9 -8 105.645 72.3456 18 -5 -10 0 260.030 77.6560 18 5 10 0 313.364 89.0544 22 5 10 1 259.850 86.3475 32 -5 -10 -1 240.300 75.0649 18 5 10 1 259.992 86.3947 22 5 10 2 3099.77 289.810 32 5 10 2 3135.89 291.316 22 -5 -10 -2 3270.79 278.674 18 5 10 3 1280.12 185.771 32 -5 -10 -3 1412.42 187.580 18 5 10 3 1289.78 186.005 22 5 10 4 25.3671 39.4444 24 5 10 4 62.1461 55.2080 32 -5 -10 -4 35.9261 49.9576 18 5 10 4 163.700 79.4594 22 -5 -10 -5 3061.63 287.698 18 5 10 5 2993.08 267.503 22 5 10 5 3819.22 272.146 24 5 10 5 3261.13 285.148 32 5 10 6 891.525 128.350 24 -5 -10 -6 702.959 138.676 18 -6 1 -1 518.012 112.118 20 -6 1 -1 747.566 115.326 25 -6 1 -1 436.954 102.992 35 -6 1 -2 5000.37 346.586 20 -6 1 -2 5089.94 304.039 25 -6 1 -2 4214.20 321.481 35 -6 1 -3 1231.91 148.935 25 -6 0 -1 1386.88 180.542 20 -6 0 -1 1389.59 154.717 25 -6 0 -1 1005.20 155.729 35 -6 0 -2 5679.97 381.996 20 -6 0 -2 4972.29 358.355 35 -6 0 -3 2595.52 249.829 20 -6 0 -3 2202.08 198.602 25 -6 0 -3 2147.55 224.953 35 -6 0 -4-5.87080 44.2037 25 -6 -1 0 284.470 86.0603 35 -6 -1 -1 4028.32 315.074 20 -6 -1 -1 3772.40 306.525 35 -6 -1 -2 145.124 76.3711 20 -6 -1 -2 190.296 63.6173 25 -6 -1 -2 102.395 64.3334 35 -6 -1 -3 6504.16 410.958 20 -6 -1 -3 6128.93 337.735 25 -6 -1 -3 5480.99 378.832 35 -6 -1 -4 2053.39 191.369 25 -6 -1 -4 2518.08 242.024 20 -6 -2 -1 4469.97 338.823 35 -6 -2 -1 5246.12 362.880 20 -6 -2 -2 3860.18 321.990 35 -6 -2 -2 4253.37 333.413 20 -6 -2 -3 9234.80 511.388 35 -6 -2 -3 10426.1 541.847 20 -6 -2 -4 15974.7 687.915 20 -6 -3 -1 6372.36 406.922 35 -6 -3 -1 6643.87 405.680 20 -6 -3 -2 1198.13 181.014 35 -6 -3 -2 1087.89 168.042 20 6 3 2 838.127 142.577 22 -6 -3 -3 4239.30 349.950 35 6 3 3 4951.32 339.119 22 0 0 0 0.00 0.00 0 TITL KSK_KC_65_auto in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 5.039905 14.266752 15.136989 82.4456 83.3581 85.9012 ZERR 15.00 0.000077 0.000155 0.000206 0.0010 0.0012 0.0011 LATT 1 SFAC C H N O Br UNIT 15.00 15.00 15.00 15.00 15.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 4 END ; _shelx_hkl_checksum 38655 _olex2_exptl_crystal_mounting_method yes _olex2_submission_original_sample_id SD100165 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.130 _oxdiff_exptl_absorpt_empirical_full_min 0.533 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 Br32 Br 0.27893(5) 0.38014(2) 0.15119(2) 0.03802(14) Uani 1 1 d . . . . . O3 O 1.5846(3) 0.14855(9) -0.15864(9) 0.0166(3) Uani 1 1 d . . . . . O11 O 1.4280(3) 0.07322(10) -0.39754(10) 0.0194(3) Uani 1 1 d . . . . . O25 O 1.0952(3) 0.18409(10) -0.40427(10) 0.0213(3) Uani 1 1 d . . . . . O24 O 1.1745(3) 0.07537(10) -0.05777(11) 0.0259(4) Uani 1 1 d . . . . . C19 C 1.1822(4) 0.42804(15) -0.25593(15) 0.0211(4) Uani 1 1 d . . . . . H19 H 1.017420 0.425057 -0.218517 0.025 Uiso 1 1 calc R U . . . N20 N 1.6115(4) 0.61016(12) -0.38489(14) 0.0269(4) Uani 1 1 d . . . . . C27 C 0.7521(4) 0.16728(16) 0.03985(14) 0.0211(4) Uani 1 1 d . . . . . H27 H 0.758589 0.100082 0.045267 0.025 Uiso 1 1 calc R U . . . C5 C 1.6867(4) 0.03885(13) -0.27007(13) 0.0163(4) Uani 1 1 d . . . . . C18 C 1.2697(5) 0.51583(15) -0.29341(15) 0.0238(5) Uani 1 1 d . . . . . H18 H 1.164423 0.571580 -0.281393 0.029 Uiso 1 1 calc R U . . . C6 C 1.8892(4) -0.01725(14) -0.22855(14) 0.0191(4) Uani 1 1 d . . . . . H6 H 1.932159 -0.006182 -0.171470 0.023 Uiso 1 1 calc R U . . . C14 C 1.3282(4) 0.34391(14) -0.27133(13) 0.0166(4) Uani 1 1 d . . . . . C28 C 0.5524(4) 0.21523(17) 0.08935(14) 0.0254(5) Uani 1 1 d . . . . . H28 H 0.422502 0.181424 0.129220 0.030 Uiso 1 1 calc R U . . . C26 C 0.9453(4) 0.21689(14) -0.01828(14) 0.0181(4) Uani 1 1 d . . . . . C13 C 1.3372(4) 0.16685(13) -0.27666(14) 0.0157(4) Uani 1 1 d . . . . . C10 C 1.6255(4) 0.02147(14) -0.35410(14) 0.0180(4) Uani 1 1 d . . . . . C31 C 0.9305(4) 0.31607(15) -0.02727(15) 0.0220(4) Uani 1 1 d . . . . . H31 H 1.059353 0.350267 -0.067221 0.026 Uiso 1 1 calc R U . . . C2 C 1.3615(4) 0.21476(13) -0.13666(13) 0.0159(4) Uani 1 1 d . . . . . H2 H 1.424586 0.269627 -0.111562 0.019 Uiso 1 1 calc R U . . . C17 C 1.5123(4) 0.52326(14) -0.34897(15) 0.0209(4) Uani 1 1 d . . . . . C29 C 0.5435(4) 0.31384(17) 0.08011(15) 0.0253(5) Uani 1 1 d . . . . . C16 C 1.6554(4) 0.43840(15) -0.36596(15) 0.0210(4) Uani 1 1 d . . . . . H16 H 1.817508 0.440895 -0.404843 0.025 Uiso 1 1 calc R U . . . C15 C 1.5670(4) 0.35110(14) -0.32763(14) 0.0185(4) Uani 1 1 d . . . . . H15 H 1.670870 0.295143 -0.339894 0.022 Uiso 1 1 calc R U . . . C30 C 0.7295(5) 0.36452(16) 0.02161(16) 0.0260(5) Uani 1 1 d . . . . . H30 H 0.718983 0.431779 0.015174 0.031 Uiso 1 1 calc R U . . . C9 C 1.7637(5) -0.04972(15) -0.39808(15) 0.0239(5) Uani 1 1 d . . . . . H9 H 1.721979 -0.061045 -0.455229 0.029 Uiso 1 1 calc R U . . . C1 C 1.2344(4) 0.24912(13) -0.22626(13) 0.0157(4) Uani 1 1 d . . . . . H1 H 1.034625 0.251253 -0.215313 0.019 Uiso 1 1 calc R U . . . C22 C 1.8093(5) 0.61284(16) -0.46278(17) 0.0303(5) Uani 1 1 d . . . . . H22A H 1.973302 0.576971 -0.446399 0.045 Uiso 1 1 calc R U . . . H22B H 1.849088 0.678707 -0.484231 0.045 Uiso 1 1 calc R U . . . H22C H 1.738937 0.584653 -0.510311 0.045 Uiso 1 1 calc R U . . . C7 C 2.0251(4) -0.08892(15) -0.27198(16) 0.0244(5) Uani 1 1 d . . . . . H7 H 2.160257 -0.128014 -0.244166 0.029 Uiso 1 1 calc R U . . . C8 C 1.9642(5) -0.10382(15) -0.35642(16) 0.0267(5) Uani 1 1 d . . . . . H8 H 2.062261 -0.152152 -0.386068 0.032 Uiso 1 1 calc R U . . . C21 C 1.4401(5) 0.69552(15) -0.3773(2) 0.0359(6) Uani 1 1 d . . . . . H21A H 1.287267 0.694151 -0.411534 0.054 Uiso 1 1 calc R U . . . H21B H 1.541790 0.751080 -0.400986 0.054 Uiso 1 1 calc R U . . . H21C H 1.375590 0.698976 -0.314099 0.054 Uiso 1 1 calc R U . . . C12 C 1.2694(4) 0.14623(13) -0.36105(14) 0.0168(4) Uani 1 1 d . . . . . C4 C 1.5352(4) 0.11714(13) -0.23548(13) 0.0151(4) Uani 1 1 d . . . . . C23 C 1.1612(4) 0.16131(14) -0.06838(14) 0.0185(4) Uani 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 Br32 0.02951(19) 0.0566(2) 0.03031(19) -0.02493(14) 0.00169(12) 0.00920(13) O3 0.0181(7) 0.0181(7) 0.0143(7) -0.0046(5) -0.0016(6) -0.0009(5) O11 0.0262(8) 0.0170(7) 0.0159(7) -0.0044(6) -0.0051(6) 0.0006(6) O25 0.0261(8) 0.0189(7) 0.0194(7) -0.0005(6) -0.0064(6) -0.0021(6) O24 0.0290(8) 0.0163(7) 0.0298(9) -0.0002(6) 0.0054(7) -0.0012(6) C19 0.0192(10) 0.0211(10) 0.0218(11) -0.0037(8) 0.0019(8) 0.0014(8) N20 0.0350(10) 0.0134(8) 0.0311(11) 0.0030(8) -0.0048(9) -0.0030(7) C27 0.0230(11) 0.0238(10) 0.0158(10) 0.0009(8) -0.0032(9) 0.0001(8) C5 0.0181(10) 0.0141(9) 0.0162(10) -0.0006(8) 0.0005(8) -0.0038(7) C18 0.0294(11) 0.0159(10) 0.0258(11) -0.0050(8) -0.0023(9) 0.0045(8) C6 0.0216(10) 0.0168(9) 0.0188(10) -0.0012(8) -0.0018(8) -0.0025(8) C14 0.0195(10) 0.0161(9) 0.0148(9) -0.0026(8) -0.0033(8) -0.0005(7) C28 0.0223(11) 0.0388(13) 0.0139(10) -0.0004(9) -0.0005(8) -0.0019(9) C26 0.0203(10) 0.0211(10) 0.0130(9) -0.0035(8) -0.0018(8) 0.0001(8) C13 0.0183(10) 0.0128(9) 0.0159(10) -0.0015(8) -0.0001(8) -0.0036(7) C10 0.0205(10) 0.0144(9) 0.0191(10) -0.0017(8) -0.0008(8) -0.0033(7) C31 0.0243(11) 0.0215(10) 0.0208(11) -0.0053(8) -0.0005(9) -0.0031(8) C2 0.0188(10) 0.0154(9) 0.0139(9) -0.0039(7) -0.0010(8) -0.0001(7) C17 0.0279(11) 0.0150(10) 0.0205(11) 0.0005(8) -0.0067(9) -0.0035(8) C29 0.0225(11) 0.0386(12) 0.0165(10) -0.0129(9) -0.0025(9) 0.0039(9) C16 0.0212(10) 0.0184(10) 0.0220(11) 0.0005(8) 0.0007(8) -0.0025(8) C15 0.0197(10) 0.0174(10) 0.0179(10) -0.0019(8) -0.0008(8) 0.0005(7) C30 0.0270(11) 0.0251(11) 0.0279(12) -0.0110(9) -0.0050(9) 0.0016(9) C9 0.0300(12) 0.0217(10) 0.0214(11) -0.0091(9) -0.0018(9) -0.0015(9) C1 0.0165(9) 0.0159(9) 0.0147(10) -0.0027(8) 0.0000(8) -0.0018(7) C22 0.0395(13) 0.0241(11) 0.0264(12) 0.0077(9) -0.0058(10) -0.0114(10) C7 0.0240(11) 0.0205(10) 0.0285(12) -0.0030(9) -0.0042(9) 0.0022(8) C8 0.0303(12) 0.0199(10) 0.0302(12) -0.0105(9) 0.0009(10) 0.0034(9) C21 0.0411(14) 0.0132(10) 0.0542(17) -0.0003(10) -0.0134(13) -0.0005(9) C12 0.0201(10) 0.0126(9) 0.0171(10) -0.0009(7) 0.0003(8) -0.0033(7) C4 0.0168(9) 0.0150(9) 0.0134(9) -0.0015(7) 0.0026(8) -0.0064(7) C23 0.0213(10) 0.0182(10) 0.0160(10) -0.0011(8) -0.0023(8) -0.0032(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 O3 C2 105.73(14) . . ? C10 O11 C12 122.94(16) . . ? C18 C19 H19 118.9 . . ? C18 C19 C14 122.2(2) . . ? C14 C19 H19 118.9 . . ? C17 N20 C22 118.12(19) . . ? C17 N20 C21 118.9(2) . . ? C21 N20 C22 116.0(2) . . ? C28 C27 H27 119.7 . . ? C28 C27 C26 120.5(2) . . ? C26 C27 H27 119.7 . . ? C6 C5 C4 125.80(19) . . ? C10 C5 C6 119.71(19) . . ? C10 C5 C4 114.46(18) . . ? C19 C18 H18 119.7 . . ? C19 C18 C17 120.67(19) . . ? C17 C18 H18 119.7 . . ? C5 C6 H6 120.4 . . ? C7 C6 C5 119.1(2) . . ? C7 C6 H6 120.4 . . ? C19 C14 C1 121.09(18) . . ? C15 C14 C19 117.24(18) . . ? C15 C14 C1 121.64(18) . . ? C27 C28 H28 120.4 . . ? C27 C28 C29 119.2(2) . . ? C29 C28 H28 120.4 . . ? C27 C26 C31 119.3(2) . . ? C27 C26 C23 118.27(18) . . ? C31 C26 C23 122.45(19) . . ? C12 C13 C1 128.28(17) . . ? C4 C13 C1 109.77(17) . . ? C4 C13 C12 121.57(18) . . ? O11 C10 C5 122.38(18) . . ? O11 C10 C9 116.44(18) . . ? C9 C10 C5 121.19(19) . . ? C26 C31 H31 119.8 . . ? C30 C31 C26 120.4(2) . . ? C30 C31 H31 119.8 . . ? O3 C2 H2 110.6 . . ? O3 C2 C1 106.65(15) . . ? O3 C2 C23 107.67(15) . . ? C1 C2 H2 110.6 . . ? C23 C2 H2 110.6 . . ? C23 C2 C1 110.61(16) . . ? N20 C17 C18 122.3(2) . . ? N20 C17 C16 120.7(2) . . ? C16 C17 C18 116.99(19) . . ? C28 C29 Br32 119.52(17) . . ? C30 C29 Br32 119.15(18) . . ? C30 C29 C28 121.3(2) . . ? C17 C16 H16 119.1 . . ? C15 C16 C17 121.8(2) . . ? C15 C16 H16 119.1 . . ? C14 C15 H15 119.4 . . ? C16 C15 C14 121.11(19) . . ? C16 C15 H15 119.4 . . ? C31 C30 C29 119.3(2) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C10 C9 H9 120.9 . . ? C8 C9 C10 118.3(2) . . ? C8 C9 H9 120.9 . . ? C14 C1 C2 113.03(16) . . ? C14 C1 H1 110.5 . . ? C13 C1 C14 113.81(16) . . ? C13 C1 C2 98.08(15) . . ? C13 C1 H1 110.5 . . ? C2 C1 H1 110.5 . . ? N20 C22 H22A 109.5 . . ? N20 C22 H22B 109.5 . . ? N20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C6 C7 H7 119.9 . . ? C6 C7 C8 120.2(2) . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? N20 C21 H21A 109.5 . . ? N20 C21 H21B 109.5 . . ? N20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O11 C12 C13 115.04(17) . . ? O25 C12 O11 116.70(18) . . ? O25 C12 C13 128.27(19) . . ? O3 C4 C5 122.08(18) . . ? C13 C4 O3 114.45(17) . . ? C13 C4 C5 123.45(18) . . ? O24 C23 C26 121.37(19) . . ? O24 C23 C2 119.95(19) . . ? C26 C23 C2 118.64(17) . . ? 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 Br32 C29 1.894(2) . ? O3 C2 1.453(2) . ? O3 C4 1.355(2) . ? O11 C10 1.374(2) . ? O11 C12 1.400(2) . ? O25 C12 1.210(2) . ? O24 C23 1.213(3) . ? C19 H19 0.9500 . ? C19 C18 1.385(3) . ? C19 C14 1.394(3) . ? N20 C17 1.390(3) . ? N20 C22 1.451(3) . ? N20 C21 1.451(3) . ? C27 H27 0.9500 . ? C27 C28 1.380(3) . ? C27 C26 1.400(3) . ? C5 C6 1.406(3) . ? C5 C10 1.400(3) . ? C5 C4 1.430(3) . ? C18 H18 0.9500 . ? C18 C17 1.404(3) . ? C6 H6 0.9500 . ? C6 C7 1.385(3) . ? C14 C15 1.394(3) . ? C14 C1 1.514(3) . ? C28 H28 0.9500 . ? C28 C29 1.393(3) . ? C26 C31 1.401(3) . ? C26 C23 1.494(3) . ? C13 C1 1.512(3) . ? C13 C12 1.432(3) . ? C13 C4 1.347(3) . ? C10 C9 1.389(3) . ? C31 H31 0.9500 . ? C31 C30 1.383(3) . ? C2 H2 1.0000 . ? C2 C1 1.572(3) . ? C2 C23 1.526(3) . ? C17 C16 1.402(3) . ? C29 C30 1.386(3) . ? C16 H16 0.9500 . ? C16 C15 1.384(3) . ? C15 H15 0.9500 . ? C30 H30 0.9500 . ? C9 H9 0.9500 . ? C9 C8 1.386(3) . ? C1 H1 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C7 H7 0.9500 . ? C7 C8 1.395(3) . ? C8 H8 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 Br32 C29 C30 C31 176.99(16) . . . . ? O3 C2 C1 C14 -98.20(18) . . . . ? O3 C2 C1 C13 22.03(18) . . . . ? O3 C2 C23 O24 -16.5(3) . . . . ? O3 C2 C23 C26 165.84(16) . . . . ? O11 C10 C9 C8 -179.80(19) . . . . ? C19 C18 C17 N20 -177.4(2) . . . . ? C19 C18 C17 C16 1.5(3) . . . . ? C19 C14 C15 C16 0.4(3) . . . . ? C19 C14 C1 C13 155.27(19) . . . . ? C19 C14 C1 C2 -94.0(2) . . . . ? N20 C17 C16 C15 176.9(2) . . . . ? C27 C28 C29 Br32 -177.50(16) . . . . ? C27 C28 C29 C30 0.7(3) . . . . ? C27 C26 C31 C30 0.9(3) . . . . ? C27 C26 C23 O24 -1.8(3) . . . . ? C27 C26 C23 C2 175.87(18) . . . . ? C5 C6 C7 C8 1.1(3) . . . . ? C5 C10 C9 C8 0.3(3) . . . . ? C18 C19 C14 C15 -0.9(3) . . . . ? C18 C19 C14 C1 177.2(2) . . . . ? C18 C17 C16 C15 -2.0(3) . . . . ? C6 C5 C10 O11 179.28(17) . . . . ? C6 C5 C10 C9 -0.8(3) . . . . ? C6 C5 C4 O3 3.6(3) . . . . ? C6 C5 C4 C13 -177.84(18) . . . . ? C6 C7 C8 C9 -1.6(3) . . . . ? C14 C19 C18 C17 -0.1(3) . . . . ? C28 C27 C26 C31 -1.4(3) . . . . ? C28 C27 C26 C23 178.38(19) . . . . ? C28 C29 C30 C31 -1.2(3) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? C26 C31 C30 C29 0.4(3) . . . . ? C10 O11 C12 O25 -177.22(17) . . . . ? C10 O11 C12 C13 3.2(2) . . . . ? C10 C5 C6 C7 0.1(3) . . . . ? C10 C5 C4 O3 -174.39(16) . . . . ? C10 C5 C4 C13 4.2(3) . . . . ? C10 C9 C8 C7 0.9(3) . . . . ? C31 C26 C23 O24 178.0(2) . . . . ? C31 C26 C23 C2 -4.3(3) . . . . ? C2 O3 C4 C5 -169.12(17) . . . . ? C2 O3 C4 C13 12.2(2) . . . . ? C17 C16 C15 C14 1.1(3) . . . . ? C15 C14 C1 C13 -26.7(3) . . . . ? C15 C14 C1 C2 84.1(2) . . . . ? C1 C14 C15 C16 -177.71(19) . . . . ? C1 C13 C12 O11 170.46(17) . . . . ? C1 C13 C12 O25 -9.1(3) . . . . ? C1 C13 C4 O3 3.1(2) . . . . ? C1 C13 C4 C5 -175.52(17) . . . . ? C1 C2 C23 O24 99.7(2) . . . . ? C1 C2 C23 C26 -78.0(2) . . . . ? C22 N20 C17 C18 -160.0(2) . . . . ? C22 N20 C17 C16 21.1(3) . . . . ? C21 N20 C17 C18 -10.4(3) . . . . ? C21 N20 C17 C16 170.7(2) . . . . ? C12 O11 C10 C5 -1.0(3) . . . . ? C12 O11 C10 C9 179.06(18) . . . . ? C12 C13 C1 C14 -68.6(3) . . . . ? C12 C13 C1 C2 171.75(18) . . . . ? C12 C13 C4 O3 176.56(16) . . . . ? C12 C13 C4 C5 -2.1(3) . . . . ? C4 O3 C2 C1 -21.74(18) . . . . ? C4 O3 C2 C23 97.01(17) . . . . ? C4 C5 C6 C7 -177.76(19) . . . . ? C4 C5 C10 O11 -2.6(3) . . . . ? C4 C5 C10 C9 177.30(19) . . . . ? C4 C13 C1 C14 104.24(19) . . . . ? C4 C13 C1 C2 -15.4(2) . . . . ? C4 C13 C12 O11 -1.6(3) . . . . ? C4 C13 C12 O25 178.8(2) . . . . ? C23 C26 C31 C30 -178.9(2) . . . . ? C23 C2 C1 C14 144.99(17) . . . . ? C23 C2 C1 C13 -94.78(18) . . . . ?