#------------------------------------------------------------------------------ #$Date: 2024-12-05 01:32:33 +0200 (Thu, 05 Dec 2024) $ #$Revision: 296222 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249665.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_7249665 loop_ _publ_author_name 'Zelenov, Victor Petrovich' 'Fedyanin, Ivan V.' 'Samigullina, Aida I.' 'Larin, Alexander' 'Sheremetev, Aleksei B.' _publ_section_title ; R-substituent vs exocyclic oxygen: influence on synthesis and crystal packing of R-[1,2,5]oxadiazolo[3,4-c]cinnoline mono- and dioxides ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE01068J _journal_year 2024 _chemical_formula_moiety 'C8 H3 Br N4 O3' _chemical_formula_sum 'C8 H3 Br N4 O3' _chemical_formula_weight 283.05 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method 'Modified SHELXL output' _audit_update_record ; 2024-06-24 deposited with the CCDC. 2024-12-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.2790(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.14290(3) _cell_length_b 8.10668(5) _cell_length_c 17.96048(8) _cell_measurement_reflns_used 16938 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 79.3890 _cell_measurement_theta_min 4.8920 _cell_volume 892.941(8) _computing_cell_refinement 'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 43.103a 64-bit (release 20-12-2023))' _computing_data_reduction 'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 8.00 122.00 0.50 0.05 -- 40.59 29.00-166.00 228 2 \w 15.00 115.00 0.50 0.05 -- 40.59 57.00 -90.00 200 3 \w 15.00 115.00 0.50 0.05 -- 40.59 57.00 -30.00 200 4 \w 110.00 140.00 0.50 0.05 -- 119.50 111.00 150.00 60 5 \w 63.00 122.00 0.50 0.05 -- 40.59 178.00 90.00 118 6 \w 63.00 122.00 0.50 0.05 -- 40.59 178.00 0.00 118 7 \w 72.00 98.00 0.50 0.05 -- 119.50 178.00-150.00 52 8 \w 67.00 133.00 0.50 0.05 -- 119.50 178.00-180.00 132 9 \w 103.00 178.00 0.50 0.05 -- 119.50 111.00-120.00 150 10 \w 117.00 143.00 0.50 0.05 -- 119.50 111.00 0.00 52 11 \w 140.00 171.00 0.50 0.05 -- 119.50 111.00 30.00 62 12 \w 147.00 173.00 0.50 0.05 -- 119.50 111.00 60.00 52 13 \w 135.00 161.00 0.50 0.05 -- 119.50 77.00 -90.00 52 14 \w 92.00 137.00 0.50 0.05 -- 119.50 77.00 -30.00 90 15 \w 87.00 114.00 0.50 0.05 -- 119.50 77.00 -90.00 54 16 \w 95.00 128.00 0.50 0.05 -- 119.50 77.00-150.00 66 17 \w 87.00 157.00 0.50 0.05 -- 119.50 77.00-120.00 140 18 \w 153.00 178.00 0.50 0.05 -- 119.50 77.00-150.00 50 19 \w 92.00 140.00 0.50 0.05 -- 119.50 77.00 -60.00 96 20 \w 95.00 121.00 0.50 0.05 -- 119.50 61.00-120.00 52 21 \w 97.00 139.00 0.50 0.05 -- 119.50 61.00 -60.00 84 22 \w 101.00 127.00 0.50 0.05 -- 119.50 61.00 -90.00 52 23 \w 97.00 129.00 0.50 0.05 -- 119.50 61.00 0.00 64 24 \w 134.00 173.00 0.50 0.05 -- 119.50 45.00 -30.00 78 25 \w 149.00 174.00 0.50 0.05 -- 119.50 61.00 0.00 50 26 \w 102.00 127.00 0.50 0.05 -- 119.50 45.00 -30.00 50 27 \w 96.00 150.00 0.50 0.05 -- 119.50 45.00 60.00 108 28 \w 92.00 117.00 0.50 0.05 -- 119.50 77.00 150.00 50 29 \w 125.00 167.00 0.50 0.05 -- 119.50 77.00 150.00 84 30 \w 87.00 178.00 0.50 0.05 -- 119.50 30.00 30.00 182 31 \w 73.00 99.00 0.50 0.05 -- 119.50 17.00 8.75 52 32 \w 53.00 79.00 0.50 0.05 -- 119.50 8.00 17.88 52 33 \w 42.00 178.00 0.50 0.05 -- 119.50 15.00-120.00 272 34 \w 87.00 178.00 0.50 0.05 -- 119.50 29.00-166.00 182 35 \w 42.00 67.00 0.50 0.05 -- 119.50 15.00-120.00 50 36 \w 91.00 150.00 0.50 0.05 -- 119.50 -79.00 -90.17 118 37 \w 67.00 104.00 0.50 0.05 -- 119.50 -77.00 -90.00 74 38 \w 46.00 76.00 0.50 0.05 -- 119.50 -77.00 0.00 60 39 \w 47.00 95.00 0.50 0.05 -- 119.50 -77.00-180.00 96 40 \w -41.00 34.00 0.50 0.05 -- 40.59 -29.00 32.00 150 41 \w 56.00 82.00 0.50 0.05 -- 119.50 -77.00 90.00 52 42 \w 49.00 79.00 0.50 0.05 -- 119.50 -77.00 150.00 60 43 \w 49.00 99.00 0.50 0.05 -- 119.50 -77.00 120.00 100 44 \w 121.00 156.00 0.50 0.05 -- 119.50 -84.00 166.67 70 45 \w 46.00 72.00 0.50 0.05 -- 119.50-111.00 150.00 52 46 \w 52.00 108.00 0.50 0.05 -- 119.50-111.00 90.00 112 47 \w 61.00 87.00 0.50 0.05 -- 119.50 -95.00 90.00 52 48 \w 74.00 108.00 0.50 0.05 -- 119.50-111.00 150.00 68 49 \w 41.00 105.00 0.50 0.05 -- 119.50 -95.00 -30.00 128 50 \w 79.00 104.00 0.50 0.05 -- 119.50-111.00 -60.00 50 51 \w 49.00 76.00 0.50 0.05 -- 119.50-111.00 -60.00 54 52 \w 41.00 67.00 0.50 0.05 -- 119.50 -95.00-150.00 52 53 \w 44.00 84.00 0.50 0.05 -- 119.50 -95.00-120.00 80 54 \w 124.00 155.00 0.50 0.05 -- 119.50 -86.00 1.97 62 55 \w -122.00 -8.00 0.50 0.05 -- -40.59 -29.00 32.00 228 56 \w -71.00 -23.00 0.50 0.05 -- -98.00 61.00 0.00 96 57 \w -34.00 42.00 0.50 0.05 -- -40.59 29.00-166.00 152 58 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -90.00 214 59 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -97.42 214 60 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -90.00 214 61 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -60.00 214 62 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -30.00 214 63 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -30.00 214 64 \w -172.00 -68.00 0.50 0.05 -- -98.00 -69.00 -21.33 208 65 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 0.00 214 66 \w -172.00 -65.00 0.50 0.05 -- -98.00 -77.00 -60.00 214 67 \w -172.00 -68.00 0.50 0.05 -- -98.00 -70.00 -84.81 208 68 \w -172.00 -65.00 0.50 0.05 -- -98.00 -76.00-125.94 214 69 \w -172.00 -70.00 0.50 0.05 -- -98.00 -63.00 -63.34 204 70 \w -172.00 -71.00 0.50 0.05 -- -98.00 -61.00 -90.00 202 71 \w -172.00 -70.00 0.50 0.05 -- -98.00 -65.00 -55.88 204 72 \w -172.00 -71.00 0.50 0.05 -- -98.00 -61.00 0.00 202 73 \w -175.00 -71.00 0.50 0.05 -- -98.00 -47.00-132.29 208 74 \w -177.00 -71.00 0.50 0.05 -- -98.00 -43.00 -64.67 212 75 \w -177.00 -65.00 0.50 0.05 -- -98.00 -29.00 32.00 224 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_method '\w scans' _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 0.0324 _diffrn_reflns_av_unetI/netI 0.0131 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 22531 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.728 _diffrn_reflns_theta_min 4.933 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.327 _exptl_absorpt_correction_T_max 0.861 _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 552 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.230 _exptl_crystal_size_min 0.170 _refine_diff_density_max 0.478 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.068 _refine_ls_extinction_coef 0.0059(2) _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 1.180 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 146 _refine_ls_number_reflns 1935 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.180 _refine_ls_R_factor_all 0.0220 _refine_ls_R_factor_gt 0.0220 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.0428P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0524 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1931 _reflns_number_total 1935 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce01068j2.cif _cod_data_source_block 1i_z483101 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7249665 _publ_contact_name 'Aida I. Samigullina' _publ_contact_email s_aida_88@mail.ru _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_min 0.280 _shelx_estimated_absorpt_t_max 0.413 _shelx_res_file ; TITL 1i_z483101 in P2(1)/n 1i_z483101.res created by SHELXL-2018/3 at 15:17:43 on 22-May-2024 CELL 1.54184 6.1429 8.10668 17.96048 90 93.279 90 ZERR 4 0.00003 0.00005 0.00008 0 0.0005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br N O UNIT 32 12 4 16 12 L.S. 10 PLAN 20 SIZE 0.17 0.23 0.27 TEMP -173 CONF BOND $H LIST 4 MORE -1 FMAP 2 53 ACTA WGHT 0.019500 1.042800 EXTI 0.005918 FVAR 0.62603 BR8 3 0.287776 0.157364 0.531901 11.00000 0.01888 0.01734 = 0.01471 0.00324 0.00369 0.00016 O1 5 0.100313 0.278940 0.228638 11.00000 0.01430 0.01593 = 0.02053 -0.00051 -0.00112 -0.00255 O2 5 0.308080 0.418951 0.145733 11.00000 0.01897 0.01731 = 0.01330 0.00153 -0.00047 0.00109 O5 5 1.018107 0.572282 0.338230 11.00000 0.01365 0.01881 = 0.02536 -0.00018 -0.00055 -0.00520 N1 4 0.268606 0.356715 0.220171 11.00000 0.01726 0.01172 = 0.01308 0.00071 0.00029 0.00262 N3 4 0.508577 0.496490 0.148443 11.00000 0.01758 0.01637 = 0.01707 0.00195 0.00218 0.00244 N4 4 0.782087 0.549137 0.242530 11.00000 0.01662 0.01417 = 0.01806 0.00195 0.00362 0.00099 N5 4 0.838268 0.518620 0.312079 11.00000 0.01383 0.01222 = 0.01897 -0.00095 0.00227 0.00005 C3A 1 0.584262 0.484087 0.218331 11.00000 0.01765 0.01013 = 0.01549 0.00020 0.00260 0.00374 C5A 1 0.707953 0.426770 0.363012 11.00000 0.01493 0.01113 = 0.01558 -0.00074 0.00281 -0.00005 C6 1 0.795141 0.397329 0.434965 11.00000 0.01485 0.01482 = 0.01787 -0.00244 -0.00144 -0.00107 AFIX 43 H6 2 0.938642 0.432970 0.449517 11.00000 -1.20000 AFIX 0 C7 1 0.670488 0.315483 0.485177 11.00000 0.01950 0.01724 = 0.01457 0.00009 -0.00144 0.00150 AFIX 43 H7 2 0.727913 0.294264 0.534483 11.00000 -1.20000 AFIX 0 C8 1 0.459537 0.264363 0.462719 11.00000 0.01737 0.01061 = 0.01705 0.00108 0.00449 0.00003 C9 1 0.372585 0.289086 0.390832 11.00000 0.01379 0.01157 = 0.01635 -0.00093 0.00159 0.00039 AFIX 43 H9 2 0.229869 0.251621 0.376337 11.00000 -1.20000 AFIX 0 C9A 1 0.498802 0.370148 0.340092 11.00000 0.01492 0.00930 = 0.01443 -0.00155 0.00071 0.00109 C9B 1 0.440702 0.399912 0.263174 11.00000 0.01311 0.00970 = 0.01578 -0.00065 0.00098 0.00129 HKLF 4 REM 1i_z483101 in P2(1)/n REM wR2 = 0.0524, GooF = S = 1.180, Restrained GooF = 1.180 for all data REM R1 = 0.0220 for 1931 Fo > 4sig(Fo) and 0.0220 for all 1935 data REM 146 parameters refined using 0 restraints END WGHT 0.0195 1.0428 REM Highest difference peak 0.478, deepest hole -0.323, 1-sigma level 0.068 Q1 1 0.3839 0.1621 0.4965 11.00000 0.05 0.48 Q2 1 0.5209 0.4433 0.2422 11.00000 0.05 0.42 Q3 1 0.1856 0.1420 0.5626 11.00000 0.05 0.37 Q4 1 0.5988 0.4198 0.3563 11.00000 0.05 0.35 Q5 1 0.4605 0.3829 0.3005 11.00000 0.05 0.32 Q6 1 0.7581 0.4853 0.3408 11.00000 0.05 0.32 Q7 1 0.5472 0.3199 0.4768 11.00000 0.05 0.32 Q8 1 0.4357 0.3357 0.3660 11.00000 0.05 0.30 Q9 1 0.7235 0.3637 0.4618 11.00000 0.05 0.30 Q10 1 0.7304 0.4127 0.3991 11.00000 0.05 0.26 Q11 1 0.3755 0.3410 0.2399 11.00000 0.05 0.25 Q12 1 0.8478 0.5830 0.2195 11.00000 0.05 0.25 Q13 1 0.0449 0.3252 0.2525 11.00000 0.05 0.24 Q14 1 0.3465 0.4019 0.2530 11.00000 0.05 0.24 Q15 1 0.4008 0.3003 0.4337 11.00000 0.05 0.23 Q16 1 0.1740 0.3346 0.2347 11.00000 0.05 0.22 Q17 1 0.5607 0.4572 0.1798 11.00000 0.05 0.22 Q18 1 0.4212 0.2672 0.4250 11.00000 0.05 0.21 Q19 1 0.6851 0.4940 0.2269 11.00000 0.05 0.21 Q20 1 0.5329 0.5183 0.1951 11.00000 0.05 0.21 ; _shelx_res_checksum 35371 _shelx_hkl_file ; 0 0 -1 5.49 0.58 0 0 -2 15.40 1.35 0 0 2 37.52 2.01 0 0 -3 0.67 0.38 0 0 3 2.15 0.61 0 0 -4 3053.73 26.82 0 0 4 3075.14 14.78 0 0 5 7.47 0.75 0 0 5 4.98 1.21 0 0 -6 1385.32 22.21 0 0 6 1348.36 9.25 0 0 6 1361.20 20.96 0 0 6 1353.37 24.65 0 0 -7 0.53 0.59 0 0 7 0.68 0.76 0 0 8 576.46 15.65 0 0 -8 608.33 17.06 0 0 8 568.93 19.09 0 0 9 1.43 0.92 0 0 9 4.95 1.12 0 0 -10 3469.43 46.30 0 0 10 3321.20 52.07 0 0 10 3336.38 42.12 0 0 11 2.87 1.58 0 0 11 0.62 0.80 0 0 11 5.11 2.28 0 0 11 0.25 0.53 0 0 11 2.51 1.49 0 0 11 1.55 1.23 0 0 -11 3.81 1.70 0 0 12 919.96 27.34 0 0 12 869.24 29.87 0 0 12 924.86 27.54 0 0 12 876.60 26.93 0 0 12 905.81 25.17 0 0 12 893.61 24.86 0 0 12 909.78 27.11 0 0 12 923.62 26.78 0 0 12 902.55 27.01 0 0 12 939.66 27.57 0 0 -12 1008.32 27.70 0 0 12 894.29 27.09 0 0 12 899.28 27.21 0 0 12 934.78 25.49 0 0 12 888.46 23.54 0 0 12 936.82 27.98 0 0 13 0.38 0.80 0 0 13 0.48 1.25 0 0 13 2.98 1.77 0 0 13 1.14 1.39 0 0 13 2.61 1.77 0 0 13 4.49 2.10 0 0 13 0.32 0.47 0 0 13 1.91 1.26 0 0 13 0.95 1.06 0 0 13 1.11 1.24 0 0 13 3.35 1.93 0 0 13 3.18 1.84 0 0 13 0.37 0.79 0 0 -13 0.36 0.54 0 0 13 0.57 0.75 0 0 13 0.38 0.81 0 0 14 792.74 27.52 0 0 14 818.76 28.13 0 0 14 784.29 30.87 0 0 14 833.86 26.04 0 0 14 797.95 28.02 0 0 14 801.74 25.31 0 0 14 810.03 25.37 0 0 14 815.96 27.70 0 0 14 779.71 27.26 0 0 14 834.38 27.09 0 0 14 800.79 27.40 0 0 14 797.77 27.52 0 0 14 849.05 28.34 0 0 14 806.02 27.95 0 0 -14 809.86 27.30 0 0 15 2.54 1.68 0 0 15 1.88 1.87 0 0 15 0.42 0.64 0 0 15 13.94 3.87 0 0 -15 0.40 1.03 0 0 15 0.42 0.90 0 0 15 1.26 1.41 0 0 15 0.43 0.91 0 0 15 0.43 0.64 0 0 15 0.85 1.10 0 0 15 0.55 1.17 0 0 15 3.82 1.88 0 0 15 3.49 1.74 0 0 15 -0.42 0.63 0 0 15 13.68 3.78 0 0 15 1.56 1.43 0 0 15 11.60 3.46 0 0 -15 2.34 1.72 0 0 -15 2.50 1.65 0 0 15 1.01 1.51 0 0 16 2306.89 48.43 0 0 16 2426.87 50.28 0 0 16 2342.89 48.13 0 0 16 2356.02 49.30 0 0 16 2395.54 49.57 0 0 16 2412.80 49.89 0 0 16 2341.29 43.53 0 0 16 2412.95 44.08 0 0 16 2416.09 48.96 0 0 -16 2243.31 50.03 0 0 -16 2419.51 48.19 0 0 16 2402.65 50.66 0 0 16 2349.26 53.16 0 0 16 2373.16 46.80 0 0 16 2397.20 48.79 0 0 16 2423.03 49.94 0 0 17 3.87 2.14 0 0 17 1.33 1.63 0 0 -17 3.62 1.91 0 0 17 1.29 1.44 0 0 -17 4.20 2.22 0 0 17 2.95 2.22 0 0 17 0.86 1.12 0 0 17 3.70 2.04 0 0 17 1.13 1.27 0 0 17 5.33 2.38 0 0 17 0.41 0.88 0 0 17 2.13 1.69 0 0 17 1.75 1.61 0 0 17 0.42 1.09 0 0 17 0.46 1.37 0 0 18 620.95 24.29 0 0 -18 613.03 23.51 0 0 18 625.17 24.90 0 0 18 614.86 24.40 0 0 -18 606.56 24.87 0 0 18 605.45 25.40 0 0 18 586.08 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351.48 12.70 0 2 21 340.86 12.41 0 2 21 362.31 12.61 0 2 22 7.77 1.67 0 -2 22 7.86 1.77 0 2 22 6.52 1.37 0 -2 -22 7.85 1.67 0 3 0 1.59 0.75 0 -3 0 1.84 1.00 0 3 1 1400.90 22.57 0 3 -1 1474.04 19.89 0 3 -1 1505.11 23.01 0 -3 1 1465.59 24.97 0 -3 -1 1459.57 26.07 0 -3 -1 1516.17 26.38 0 -3 1 1345.80 25.82 0 3 2 430.20 13.47 0 3 -2 442.39 9.93 0 3 -2 451.42 11.82 0 -3 2 421.84 13.47 0 -3 -2 441.47 14.92 0 -3 2 432.28 15.08 0 -3 -2 438.05 13.82 0 3 -3 1915.35 16.61 0 -3 -3 1812.21 16.32 0 -3 3 1905.98 28.97 0 -3 -3 1826.88 32.22 0 -3 3 1987.26 32.96 0 -3 -3 1981.61 28.63 0 3 3 1967.02 30.42 0 3 -3 1989.94 22.98 0 3 -3 1946.54 18.87 0 -3 3 1910.40 17.88 0 -3 4 6.49 1.94 0 3 -4 2.85 0.84 0 3 -4 12.17 1.68 0 -3 -4 11.94 1.66 0 3 -5 1540.11 21.92 0 -3 -5 1489.66 21.50 0 -3 5 1516.66 29.75 0 3 5 1586.40 30.33 0 -3 5 1493.39 23.44 0 -3 -6 2.51 1.04 0 3 -6 1.99 0.93 0 3 6 7.59 1.99 0 3 6 2.97 1.46 0 -3 6 10.25 2.52 0 -3 7 90.19 7.48 0 -3 -7 101.48 6.92 0 3 -7 104.27 6.97 0 3 7 107.26 8.65 0 3 7 110.47 7.90 0 -3 7 104.79 7.74 0 -3 8 871.38 23.42 0 -3 8 920.94 24.66 0 3 8 1009.51 25.69 0 3 -8 988.62 22.92 0 -3 -8 925.03 22.25 0 3 8 908.19 26.19 0 3 9 97.81 8.78 0 3 9 112.55 9.21 0 -3 9 110.02 9.15 0 -3 9 104.53 9.81 0 -3 9 93.32 9.34 0 3 9 103.23 9.03 0 -3 9 109.83 10.26 0 -3 9 100.10 9.41 0 -3 9 109.18 9.87 0 3 9 104.50 9.03 0 -3 9 115.57 10.52 0 3 9 87.94 8.34 0 -3 9 93.78 7.63 0 3 9 110.23 9.16 0 -3 -9 97.18 7.74 0 3 -9 111.82 8.25 0 3 10 21.93 4.04 0 3 10 32.18 5.23 0 -3 10 24.43 4.61 0 -3 10 27.98 5.54 0 -3 10 25.47 4.92 0 -3 10 22.89 4.94 0 3 10 23.46 4.26 0 -3 10 41.11 6.53 0 3 10 24.82 4.64 0 3 10 25.64 4.54 0 -3 10 36.90 6.17 0 3 10 34.60 5.54 0 -3 10 27.78 5.12 0 3 10 22.74 4.31 0 -3 10 24.79 4.83 0 -3 10 28.22 5.36 0 -3 10 27.77 5.19 0 -3 10 17.34 4.32 0 3 10 24.79 4.73 0 3 10 24.93 4.63 0 -3 10 30.69 5.50 0 3 10 25.13 4.66 0 -3 -10 26.03 4.32 0 3 -10 23.85 4.00 0 3 10 27.09 4.60 0 3 10 25.64 4.83 0 -3 10 17.84 4.16 0 3 10 21.38 4.03 0 3 11 460.42 18.96 0 -3 11 472.62 21.31 0 3 11 471.36 21.09 0 -3 11 481.49 22.99 0 3 11 463.44 20.57 0 -3 11 458.79 21.44 0 -3 11 485.38 22.62 0 -3 11 471.17 22.42 0 3 11 456.58 19.40 0 3 11 465.09 19.73 0 -3 11 457.79 22.06 0 3 11 466.63 20.50 0 3 11 469.65 19.82 0 -3 11 486.86 21.96 0 -3 11 491.34 22.11 0 -3 11 446.78 20.93 0 -3 11 484.20 22.51 0 3 11 474.80 20.75 0 3 11 458.66 20.55 0 -3 11 491.63 23.26 0 3 11 466.05 20.78 0 -3 11 488.63 22.66 0 3 -11 485.41 18.86 0 -3 -11 482.11 19.03 0 3 11 461.92 19.36 0 3 11 461.47 20.80 0 3 11 474.13 19.71 0 -3 -11 438.81 18.01 0 3 -11 465.85 18.39 0 -3 11 471.19 21.54 0 3 12 454.47 19.40 0 -3 12 408.62 20.78 0 3 12 458.19 21.65 0 -3 12 430.18 22.15 0 3 12 453.87 20.04 0 -3 12 436.34 21.25 0 -3 12 458.42 21.84 0 -3 12 460.81 21.56 0 -3 12 446.92 21.92 0 3 12 471.13 21.19 0 -3 12 445.48 22.49 0 3 12 462.88 21.30 0 3 12 470.25 21.41 0 -3 12 458.06 22.11 0 -3 -12 456.00 19.28 0 3 -12 470.41 19.48 0 3 12 452.08 19.78 0 -3 12 453.58 21.49 0 -3 12 459.71 22.58 0 3 12 451.69 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2.22 0 3 14 5.98 2.47 0 3 14 5.65 2.61 0 -3 14 6.10 2.63 0 3 14 8.02 3.04 0 -3 14 14.79 4.02 0 3 14 3.91 2.16 0 -3 14 4.68 2.43 0 -3 14 2.20 2.02 0 3 14 3.22 2.00 0 3 14 4.46 2.28 0 3 -14 4.35 2.03 0 -3 -14 5.53 2.35 0 -3 14 3.68 2.19 0 3 15 950.90 29.05 0 -3 15 935.71 30.19 0 3 15 981.66 30.25 0 3 15 981.42 32.52 0 -3 15 1008.33 33.60 0 3 15 1013.01 30.81 0 3 15 934.26 34.52 0 -3 -15 967.01 35.47 0 3 15 993.32 31.39 0 3 15 1035.36 31.33 0 -3 15 963.53 30.86 0 -3 15 1013.55 33.15 0 3 15 989.32 31.86 0 -3 15 964.30 32.42 0 3 15 989.86 31.93 0 3 15 1001.35 32.49 0 -3 15 1017.43 34.33 0 -3 15 990.78 31.90 0 -3 15 1007.01 34.46 0 3 15 1091.43 32.12 0 -3 15 989.42 35.47 0 3 15 1012.13 30.65 0 -3 -15 999.14 29.58 0 3 -15 1024.00 29.47 0 -3 15 1010.54 33.08 0 3 15 1024.64 31.20 0 3 16 39.76 5.82 0 -3 16 29.91 5.32 0 3 16 28.88 5.17 0 3 16 24.18 5.07 0 3 16 31.18 5.39 0 -3 16 29.36 5.63 0 3 16 24.60 5.55 0 -3 -16 34.35 6.59 0 -3 16 28.33 5.15 0 -3 16 30.60 5.68 0 3 16 29.38 5.41 0 3 16 26.95 5.00 0 3 16 29.10 5.25 0 -3 16 31.87 5.75 0 3 16 32.68 5.76 0 3 16 25.40 5.13 0 -3 16 35.65 5.90 0 3 16 40.04 6.06 0 -3 16 27.37 5.72 0 -3 16 31.31 6.31 0 3 16 32.68 5.57 0 -3 16 26.38 5.41 0 -3 -16 27.30 4.82 0 3 16 31.10 5.21 0 3 -16 27.60 4.84 0 3 17 741.44 23.96 0 -3 17 685.69 24.10 0 3 17 680.66 28.04 0 -3 -17 762.82 29.49 0 3 17 744.24 25.91 0 3 17 716.39 24.44 0 3 17 698.56 24.16 0 -3 17 712.25 25.71 0 3 17 684.57 24.86 0 -3 17 695.79 25.42 0 3 17 672.02 25.15 0 -3 17 685.96 25.90 0 3 17 720.05 24.51 0 3 17 715.32 23.30 0 3 -17 692.80 23.19 0 3 17 761.73 25.45 0 -3 -17 697.07 23.39 0 -3 17 763.10 30.79 0 3 17 722.09 26.17 0 -3 17 728.08 28.75 0 -3 17 712.40 24.99 0 3 17 761.31 25.41 0 -3 17 722.84 27.69 0 3 18 234.27 13.22 0 -3 18 233.13 14.91 0 3 18 231.93 13.98 0 3 18 239.26 13.27 0 3 18 231.70 13.81 0 -3 18 239.64 14.14 0 3 18 227.88 13.17 0 3 -18 243.63 12.86 0 3 18 256.62 14.62 0 -3 18 234.74 16.06 0 -3 -18 255.93 15.91 0 3 18 235.15 15.46 0 3 18 247.87 13.37 0 3 18 236.90 13.17 0 3 18 229.17 13.48 0 3 18 227.22 13.48 0 -3 18 245.07 15.58 0 -3 -18 262.41 16.81 0 3 18 245.24 12.82 0 3 19 725.23 21.11 0 3 19 714.84 22.26 0 -3 19 758.39 25.97 0 3 19 730.15 21.44 0 3 -19 708.61 19.80 0 3 19 706.01 22.18 0 3 19 716.03 20.90 0 -3 19 789.25 26.83 0 3 19 775.90 23.31 0 3 19 767.85 25.73 0 3 19 712.67 20.80 0 3 19 725.22 21.55 0 3 19 720.95 21.58 0 -3 19 783.84 25.34 0 -3 -19 799.96 26.83 0 3 19 718.98 19.61 0 3 20 13.02 2.68 0 3 20 9.00 2.08 0 3 20 9.40 2.60 0 3 20 9.07 2.12 0 3 20 9.77 2.13 0 3 20 11.74 2.39 0 -3 -20 17.47 3.58 0 3 20 6.74 1.86 0 3 20 7.82 2.13 0 -3 20 12.29 2.95 0 3 20 9.51 2.19 0 3 20 7.05 2.02 0 -3 20 11.34 2.82 0 -3 20 9.40 2.48 0 3 20 10.70 2.43 0 -3 21 96.76 6.41 0 3 21 102.79 6.93 0 3 21 100.07 5.98 0 -3 -21 105.69 7.12 0 4 0 904.46 19.57 0 4 0 848.65 21.83 0 -4 0 821.83 22.76 0 -4 0 856.02 24.14 0 4 1 593.18 17.05 0 4 -1 616.16 15.12 0 4 -1 586.29 17.21 0 4 1 599.00 18.97 0 -4 -1 568.94 19.38 0 -4 1 584.17 18.84 0 -4 -1 569.49 19.30 0 4 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855.64 26.50 0 4 9 889.83 25.67 0 -4 9 951.86 32.52 0 4 9 943.04 30.04 0 4 9 925.38 29.84 0 4 9 914.32 26.03 0 -4 9 952.50 31.52 0 4 9 924.15 27.27 0 4 9 902.11 28.70 0 4 10 367.73 18.87 0 -4 10 396.35 21.09 0 4 10 398.36 18.47 0 4 10 394.13 19.70 0 4 10 370.26 19.54 0 -4 10 431.74 22.93 0 -4 10 387.04 20.95 0 -4 10 394.17 20.77 0 -4 10 411.55 21.56 0 4 10 383.36 17.49 0 -4 10 397.30 21.92 0 4 10 368.66 17.88 0 4 10 385.50 17.42 0 -4 10 409.07 21.75 0 -4 10 420.85 22.07 0 4 10 395.38 19.64 0 4 10 387.24 17.97 0 -4 10 399.72 20.37 0 4 11 918.64 28.75 0 -4 11 919.74 33.31 0 4 11 920.77 30.43 0 4 11 843.45 28.88 0 -4 11 933.56 34.81 0 4 11 917.14 28.77 0 4 11 904.76 30.45 0 -4 11 907.25 33.03 0 -4 11 905.96 34.40 0 -4 11 914.10 33.06 0 -4 11 928.07 32.35 0 4 11 882.37 27.38 0 4 11 918.85 27.33 0 -4 11 888.06 31.27 0 4 11 863.63 27.54 0 -4 11 938.66 34.10 0 -4 11 1000.04 35.26 0 4 11 929.34 30.70 0 -4 12 123.08 13.22 0 4 12 122.27 10.36 0 4 12 122.95 10.17 0 4 12 115.11 10.85 0 4 12 106.88 10.18 0 4 12 115.21 11.19 0 -4 12 118.03 12.17 0 4 12 114.02 10.92 0 4 12 109.16 9.91 0 -4 12 120.15 12.33 0 -4 12 131.45 12.01 0 -4 12 123.53 12.28 0 4 12 114.49 10.29 0 4 12 111.11 10.83 0 -4 12 119.32 12.40 0 -4 12 117.70 12.24 0 4 12 113.10 10.22 0 -4 12 127.81 12.36 0 -4 12 114.53 12.25 0 4 12 116.36 11.07 0 4 12 97.09 10.11 0 -4 12 123.51 11.75 0 -4 12 121.52 12.06 0 4 12 118.82 11.25 0 -4 -12 105.49 12.24 0 -4 12 114.68 11.03 0 4 12 116.84 11.91 0 -4 13 950.04 36.36 0 4 13 971.77 28.64 0 4 13 1012.87 33.39 0 -4 13 932.14 35.48 0 4 13 963.25 31.59 0 4 13 973.69 29.63 0 -4 13 950.87 34.17 0 4 13 940.05 29.33 0 4 13 986.96 32.49 0 -4 13 953.42 31.88 0 4 13 999.65 32.58 0 -4 13 1005.20 34.58 0 4 13 940.47 29.48 0 -4 13 977.54 35.66 0 -4 13 860.67 28.87 0 -4 13 923.57 34.18 0 4 13 968.64 29.99 0 4 13 994.82 32.46 0 4 13 1013.65 33.10 0 -4 13 1012.00 34.52 0 -4 13 976.37 35.42 0 -4 13 937.05 31.80 0 4 13 1023.19 33.18 0 -4 13 968.04 33.63 0 -4 -13 927.59 36.27 0 -4 13 877.16 30.67 0 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3.08 0 4 15 8.48 3.12 0 -4 -15 8.61 3.45 0 -4 15 4.97 2.87 0 4 15 2.55 1.73 0 4 16 410.81 17.09 0 -4 16 451.44 24.38 0 -4 16 423.65 22.50 0 4 16 451.69 20.85 0 4 16 425.49 17.80 0 -4 16 409.41 20.06 0 4 16 438.31 18.83 0 4 16 414.21 19.88 0 -4 16 376.74 17.62 0 4 16 457.94 19.07 0 4 16 430.24 20.25 0 -4 16 421.93 21.84 0 4 16 414.05 21.64 0 -4 -16 408.73 22.42 0 4 16 443.04 18.89 0 4 16 444.56 20.36 0 -4 16 429.17 20.04 0 -4 16 409.45 21.44 0 4 16 413.95 19.19 0 -4 16 407.67 19.56 0 4 16 452.28 20.43 0 4 16 434.98 20.06 0 -4 -16 414.66 22.70 0 -4 16 405.94 22.01 0 4 16 430.27 18.42 0 4 16 418.95 18.92 0 4 17 177.59 11.21 0 4 17 157.65 11.59 0 -4 17 165.86 13.18 0 -4 -17 175.74 13.88 0 4 17 157.34 12.54 0 4 17 181.33 12.12 0 4 17 188.92 11.57 0 4 17 164.01 11.22 0 -4 17 173.57 13.17 0 4 17 153.55 11.23 0 -4 -17 177.30 14.05 0 4 17 168.05 11.80 0 4 17 186.65 11.52 0 -4 17 165.36 13.90 0 -4 17 175.35 13.19 0 -4 17 167.55 13.27 0 4 17 170.30 10.90 0 4 17 173.96 11.26 0 4 18 185.64 10.34 0 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2337.19 44.32 0 5 5 57.55 7.08 0 5 5 72.88 8.61 0 -5 -5 74.21 9.23 0 -5 5 68.85 8.51 0 -5 -6 1833.71 46.85 0 -5 -6 1894.15 40.99 0 5 6 1942.92 45.19 0 5 6 1903.75 41.59 0 5 6 1820.99 36.64 0 5 7 73.91 7.90 0 5 7 78.99 8.78 0 -5 7 76.80 9.31 0 5 7 80.56 8.00 0 -5 7 74.35 9.08 0 -5 7 79.83 9.31 0 -5 -7 60.29 8.85 0 -5 7 66.67 8.55 0 -5 7 69.33 7.76 0 5 7 76.54 8.06 0 5 8 922.58 28.26 0 5 8 971.26 31.60 0 5 8 958.94 32.89 0 -5 8 968.78 33.23 0 5 8 935.11 27.70 0 -5 8 950.98 32.93 0 -5 8 984.72 33.27 0 -5 8 819.78 29.55 0 -5 -8 930.05 35.53 0 5 8 958.38 28.98 0 5 9 58.77 7.33 0 -5 9 61.71 8.65 0 -5 9 52.63 7.88 0 -5 9 49.57 7.81 0 5 9 57.78 8.11 0 5 9 55.39 7.77 0 5 9 53.19 7.43 0 5 9 52.79 6.73 0 5 9 48.12 6.63 0 5 9 55.87 7.61 0 -5 -9 61.83 9.46 0 -5 9 47.87 7.06 0 5 10 1975.02 47.02 0 5 10 2053.92 48.30 0 -5 10 2036.69 47.36 0 5 10 2194.63 45.04 0 5 10 2261.13 48.95 0 5 10 2173.63 48.14 0 5 10 2129.59 43.00 0 -5 10 2093.99 56.57 0 -5 10 2120.31 53.04 0 5 10 2214.20 45.25 0 -5 10 2122.55 51.11 0 5 10 2047.22 47.39 0 5 10 2111.54 48.20 0 -5 10 2146.39 50.41 0 -5 10 2129.79 51.18 0 -5 -10 2006.63 54.89 0 -5 10 1973.69 54.32 0 -5 -10 2100.34 54.71 0 -5 -10 2181.36 56.51 0 -5 11 471.76 23.01 0 5 11 521.44 23.84 0 5 11 505.27 21.75 0 -5 11 532.94 25.73 0 5 11 523.80 22.74 0 5 11 517.91 23.70 0 5 11 487.28 20.62 0 -5 11 488.68 27.82 0 -5 11 481.31 21.62 0 5 11 503.36 21.71 0 -5 11 502.32 25.17 0 5 11 510.81 24.02 0 -5 11 517.74 25.54 0 -5 11 514.86 24.56 0 -5 11 462.32 26.63 0 -5 -11 526.89 28.24 0 -5 -11 477.33 26.81 0 -5 12 588.32 25.64 0 5 12 653.34 26.74 0 5 12 653.13 24.52 0 -5 12 606.11 27.01 0 5 12 625.47 25.02 0 5 12 654.38 23.78 0 5 12 653.23 26.61 0 -5 12 582.91 30.12 0 -5 12 603.59 24.16 0 5 12 648.38 24.52 0 5 12 638.92 26.54 0 -5 12 590.56 26.69 0 -5 12 615.46 26.56 0 -5 12 587.47 26.62 0 -5 12 624.85 30.69 0 -5 -12 620.36 30.41 0 -5 -12 631.26 30.65 0 -5 13 173.63 13.71 0 -5 13 181.78 16.61 0 5 13 178.19 12.23 0 5 13 190.44 14.31 0 5 13 213.52 15.09 0 5 13 169.31 12.92 0 5 13 171.14 12.30 0 5 13 182.34 13.89 0 -5 13 168.53 12.46 0 -5 13 170.52 14.81 0 5 13 183.73 12.71 0 5 13 184.11 14.05 0 -5 13 186.37 14.52 0 -5 13 181.03 13.82 0 -5 13 182.22 14.36 0 -5 13 180.20 16.11 0 -5 -13 166.07 15.36 0 -5 -13 175.95 15.85 0 5 14 22.01 5.00 0 -5 14 18.64 4.07 0 -5 14 19.19 4.98 0 5 14 14.18 3.49 0 -5 -14 14.44 4.67 0 5 14 16.19 4.28 0 -5 14 21.90 4.79 0 5 14 17.89 4.24 0 5 14 19.50 4.09 0 5 14 15.89 4.16 0 -5 14 17.93 4.35 0 5 14 14.90 4.04 0 -5 14 22.69 5.65 0 5 14 16.64 4.19 0 5 14 12.45 3.59 0 5 14 14.70 3.82 0 5 14 16.55 4.22 0 5 14 15.54 3.59 0 -5 -14 13.75 4.47 0 5 15 130.06 9.61 0 5 15 123.78 10.69 0 5 15 132.50 11.11 0 5 15 145.20 11.39 0 5 15 122.53 9.60 0 5 15 132.82 11.13 0 -5 -15 126.36 12.49 0 5 15 143.00 11.11 0 5 15 137.85 11.31 0 5 15 131.92 11.00 0 5 15 128.35 9.84 0 5 15 125.90 11.35 0 -5 15 123.61 12.24 0 5 15 129.37 10.69 0 5 16 23.76 3.84 0 5 16 28.15 4.83 0 5 16 19.59 3.61 0 5 16 20.75 4.12 0 5 16 14.90 3.40 0 5 16 30.65 5.07 0 5 16 22.14 3.91 0 5 16 25.21 4.76 0 5 16 18.59 3.96 0 5 16 26.85 4.58 0 5 16 19.29 3.58 0 5 16 18.93 4.03 0 -5 -16 27.51 5.50 0 -5 16 27.41 5.47 0 5 16 29.32 4.76 0 5 17 4.67 1.64 0 5 17 4.70 1.94 0 5 17 5.78 1.83 0 5 17 3.64 1.68 0 5 17 5.33 1.97 0 5 17 6.56 2.08 0 5 17 7.25 2.34 0 -5 17 5.29 2.52 0 5 17 4.30 1.87 0 -5 17 1.82 1.55 0 5 17 4.71 1.93 0 5 17 5.20 1.87 0 5 18 99.13 7.35 0 -5 18 91.44 8.31 0 5 18 110.48 7.85 0 5 18 94.13 7.01 0 -5 18 101.23 8.18 0 5 18 99.81 7.05 0 5 18 98.34 7.47 0 5 18 91.24 7.12 0 5 18 91.03 6.88 0 5 19 8.79 1.97 0 5 19 4.67 1.35 0 -5 19 6.90 2.06 0 5 20 447.34 9.91 0 -5 20 433.94 10.61 0 -6 0 768.76 28.75 0 -6 0 756.86 26.49 0 6 0 795.17 26.21 0 -6 -1 122.65 11.74 0 -6 1 107.18 11.30 0 -6 1 128.41 11.60 0 -6 -1 133.98 12.38 0 -6 -1 115.87 10.61 0 -6 1 133.97 10.93 0 6 -1 138.85 10.51 0 6 1 129.37 11.01 0 -6 -2 1184.25 37.43 0 -6 2 1218.98 35.04 0 -6 2 1243.59 33.02 0 -6 -2 1268.78 35.13 0 6 2 1294.90 35.95 0 -6 -3 3.15 2.08 0 -6 -3 2.10 1.66 0 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1387.67 42.66 0 -7 1 1435.76 44.28 0 -7 -1 1435.78 44.64 0 -7 1 1484.72 37.92 0 -7 -1 1521.07 39.71 0 -7 -2 243.21 16.18 0 -7 2 269.90 15.74 0 -7 2 257.23 17.31 0 -7 -2 275.18 19.71 0 -7 2 260.17 18.40 0 -7 2 241.88 15.52 0 -7 -2 301.87 18.88 0 -7 2 257.11 17.26 0 -7 -2 282.63 17.80 0 -7 2 256.06 17.38 0 -7 2 269.92 17.84 0 -7 -2 254.73 18.22 0 -7 -2 272.93 18.15 0 -7 -2 272.28 19.51 0 -7 2 259.93 18.73 0 -7 -3 475.66 22.78 0 -7 3 488.54 24.02 0 -7 -3 475.07 22.81 0 -7 -3 472.27 24.98 0 -7 -3 462.07 23.61 0 -7 3 462.94 23.36 0 -7 -3 509.77 26.84 0 -7 3 475.16 23.30 0 -7 3 454.56 23.21 0 -7 -3 435.23 25.15 0 -7 3 465.78 22.41 0 -7 -3 491.17 24.13 0 -7 4 228.86 15.56 0 -7 4 214.11 15.93 0 -7 -4 199.16 16.48 0 -7 4 192.43 14.94 0 -7 -4 205.56 14.80 0 -7 -4 226.07 16.37 0 -7 4 215.83 16.36 0 -7 4 194.22 14.75 0 -7 -4 224.52 18.25 0 -7 -5 165.82 14.03 0 -7 5 174.31 13.25 0 -7 5 178.94 14.28 0 -7 -5 186.82 16.16 0 -7 -5 188.06 14.80 0 -7 5 180.83 14.68 0 -7 -5 166.20 15.91 0 -7 5 184.72 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571.29 18.22 -6 5 -2 527.15 16.87 -6 5 -2 595.65 19.96 -6 -5 -2 613.89 20.30 -6 -5 -2 606.61 17.84 -6 5 -2 555.98 17.74 -6 5 -2 576.41 18.11 -6 5 -3 4.60 1.57 -6 5 -3 2.65 1.54 -6 5 -3 4.01 1.80 6 -5 3 3.52 1.51 -6 -5 -3 3.91 1.78 -6 -5 -3 5.01 1.90 -6 5 -3 1.82 1.08 -6 5 -3 5.38 2.06 -6 5 -3 4.78 1.52 -6 5 -3 5.59 1.82 -6 5 -4 162.24 9.13 -6 5 -4 189.48 10.32 -6 5 -4 199.09 10.80 6 -5 4 172.24 9.94 -6 -5 -4 188.86 10.68 -6 -5 -4 190.83 10.30 -6 5 -4 168.88 9.19 -6 5 -4 178.01 9.61 -6 5 -4 187.12 10.60 6 -5 5 13.03 2.70 -6 -5 -5 13.34 2.80 -6 -5 -5 12.19 2.44 -6 5 -5 15.11 2.83 -6 5 -5 11.85 2.40 -6 5 -5 19.23 3.27 -6 5 -5 10.61 2.37 -6 5 -6 26.76 3.25 -6 -5 -6 28.30 3.61 -6 5 -6 31.31 3.84 -6 -5 -6 26.03 3.11 -6 -5 -7 145.41 5.51 -6 -5 -7 182.76 7.68 -6 5 -7 161.21 6.40 -6 5 -7 189.14 8.40 -6 5 -7 194.21 8.84 6 5 8 126.53 5.63 -6 5 -8 127.72 6.31 -6 5 -8 123.80 5.68 6 -5 8 116.49 5.36 -6 6 7 21.18 2.28 -6 6 7 20.54 2.32 -6 -6 7 24.52 2.63 -6 6 6 748.41 14.56 -6 6 6 717.73 15.12 -6 -6 6 773.88 15.56 -6 -6 6 798.59 16.42 -6 6 5 19.82 2.52 -6 6 5 18.34 2.57 -6 -6 5 22.47 2.97 -6 -6 5 21.04 2.91 -6 6 4 429.37 12.62 -6 -6 4 463.43 13.69 -6 6 3 28.51 2.90 -6 -6 3 31.73 3.75 -6 -6 3 28.03 3.47 -6 6 3 35.41 3.67 -6 6 2 34.65 3.85 -6 6 2 22.62 2.38 -6 -6 2 31.96 3.81 -6 -6 2 34.30 3.78 -6 -6 2 32.24 3.67 -6 6 1 79.18 5.93 -6 -6 1 83.97 6.08 -6 -6 0 1.48 0.92 -6 -6 0 4.58 1.51 -6 6 0 1.56 0.78 -6 6 0 3.47 1.36 -6 -6 -1 1.50 1.05 -6 6 -1 2.42 1.13 -6 6 -1 2.58 1.20 -6 6 -1 1.48 1.07 -6 -6 -2 6.82 1.78 -6 6 -2 6.40 1.73 -6 6 -2 7.32 1.81 -6 6 -2 7.55 1.89 -6 -6 -3 72.95 5.21 -6 6 -3 69.36 5.20 -6 6 -3 77.98 5.27 -6 6 -3 73.31 5.14 -6 6 -4 364.82 10.03 -6 6 -4 354.88 10.17 -6 -6 -4 373.20 10.43 6 -6 5 165.93 6.78 7 0 -11 70.23 4.32 7 0 -10 3.75 1.13 7 0 -10 0.62 0.57 7 0 -10 3.62 1.09 7 0 -9 107.38 6.61 7 0 -9 102.03 6.33 7 0 -9 113.34 7.13 -7 0 8 0.81 0.86 7 0 -8 4.13 1.48 7 0 -8 2.44 1.26 7 0 -8 0.87 0.87 -7 0 8 0.42 0.77 -7 0 7 60.82 5.78 -7 0 7 62.35 5.75 7 0 -7 60.40 5.62 7 0 -7 57.47 5.78 7 0 -7 61.66 5.47 7 0 -7 72.80 6.27 -7 0 6 1.23 1.11 -7 0 6 1.63 1.05 7 0 -6 3.86 1.66 7 0 -6 2.56 1.39 7 0 -6 2.99 1.49 7 0 -6 1.30 1.10 -7 0 5 410.76 15.82 -7 0 5 398.58 15.06 7 0 -5 434.41 16.25 7 0 -5 446.24 17.06 7 0 -5 418.53 15.76 7 0 -5 447.04 16.76 -7 0 4 -0.26 0.68 -7 0 4 0.24 0.89 7 0 -4 1.39 1.10 7 0 -4 2.28 1.42 7 0 -4 1.34 1.28 7 0 -4 3.22 1.66 7 0 -3 297.40 14.38 7 0 -3 292.86 13.86 -7 0 3 260.58 12.73 7 0 -3 315.52 14.61 7 0 -3 273.27 13.37 -7 0 3 283.80 14.44 -7 0 2 0.78 0.78 -7 0 2 0.33 0.99 7 0 -2 0.29 0.87 7 0 -2 1.48 1.40 7 0 -1 657.81 21.02 -7 0 1 671.44 23.31 7 0 -1 661.93 21.36 7 0 -1 639.74 21.23 -7 0 0 1.58 1.34 7 0 0 2.32 1.51 7 0 0 3.23 1.71 7 0 0 -0.28 0.95 -7 0 0 1.73 1.47 7 0 1 387.58 16.27 7 0 1 387.78 15.92 -7 0 -1 383.54 17.62 7 0 1 390.42 16.15 -7 0 -1 354.34 15.78 -7 0 -1 373.62 16.80 7 0 2 3.06 1.67 -7 0 -2 0.29 0.97 -7 0 -2 3.18 1.85 -7 0 -3 274.39 13.34 7 0 3 285.41 13.33 7 0 3 278.56 13.31 -7 0 -4 1.80 1.35 7 0 4 1.25 1.12 -7 0 -4 1.03 1.02 7 0 5 81.70 6.58 -7 0 -5 92.88 7.77 -7 0 -5 89.14 7.09 7 0 5 80.28 6.71 7 0 6 0.19 0.68 -7 0 -6 0.71 0.87 7 0 6 0.42 0.63 -7 0 -6 1.69 1.05 7 0 7 81.21 5.77 7 0 7 77.19 5.05 -7 0 -7 83.86 6.21 7 0 7 80.93 5.79 7 0 7 79.20 5.86 7 0 8 0.57 0.52 7 0 8 0.73 0.62 7 0 9 11.62 1.64 7 0 9 13.71 1.80 7 0 9 13.26 1.81 7 -1 -11 392.36 9.18 7 -1 -11 401.51 9.10 7 1 -11 392.04 8.90 7 -1 -11 383.58 9.01 7 -1 -10 69.99 4.75 7 -1 -10 58.88 4.31 7 1 -10 64.07 4.53 7 -1 -10 61.53 4.47 7 1 -9 194.49 8.27 7 1 -9 176.52 7.13 7 -1 -9 222.34 9.56 7 1 -9 221.88 9.46 7 -1 -9 210.61 9.20 7 -1 -9 209.47 9.12 7 1 -9 172.21 6.95 -7 1 8 3.05 1.33 7 1 -8 3.15 1.25 7 -1 -8 4.55 1.54 7 1 -8 5.36 1.62 7 1 -8 4.24 1.36 7 -1 -8 3.66 1.43 7 1 -8 3.62 1.51 7 -1 -8 2.40 1.24 -7 -1 7 868.48 20.43 -7 1 7 882.24 21.39 7 -1 -7 917.45 21.80 7 1 -7 931.25 22.21 7 1 -7 854.74 19.45 7 -1 -7 929.09 22.19 7 1 -7 875.24 21.01 7 1 -7 892.50 20.32 7 -1 -7 934.94 22.40 -7 1 6 8.74 2.39 -7 1 6 8.90 2.28 7 1 -6 11.42 2.48 7 -1 -6 6.20 1.99 7 1 -6 12.61 2.74 7 1 -6 8.75 2.28 7 -1 -6 9.11 2.45 7 1 -6 6.83 2.07 7 -1 -6 9.22 2.42 -7 1 5 74.27 6.74 -7 1 5 74.98 6.60 7 -1 -5 79.31 6.89 7 1 -5 72.92 6.72 7 -1 -5 80.88 7.02 7 1 -5 79.05 6.52 7 -1 -5 82.38 6.63 7 1 -5 75.84 6.55 7 -1 -5 83.09 7.18 -7 1 4 93.13 7.70 -7 1 4 99.30 7.66 7 1 -4 94.83 7.80 7 -1 -4 101.00 8.05 7 -1 -4 101.76 7.63 7 1 -4 82.64 7.25 -7 1 4 103.67 8.50 7 1 -4 105.37 7.91 -7 1 3 219.91 11.87 -7 1 3 212.34 11.24 7 1 -3 242.43 12.62 7 -1 -3 224.06 12.14 7 -1 -3 225.61 11.69 7 1 -3 249.79 12.76 -7 1 3 239.08 13.34 7 1 -3 238.30 12.23 -7 1 2 270.50 13.11 7 1 -2 304.85 14.24 7 -1 -2 285.77 13.75 -7 1 2 269.08 12.49 7 -1 -2 309.76 13.91 7 1 -2 298.01 13.95 -7 1 2 300.88 15.29 7 1 -2 286.41 13.53 7 1 -1 24.95 4.12 7 -1 -1 16.54 3.31 7 1 -1 21.92 3.83 -7 1 1 21.14 3.87 -7 1 1 20.72 3.63 -7 -1 1 22.39 4.13 7 -1 -1 18.88 3.60 -7 1 1 19.52 4.01 7 1 -1 12.93 3.01 7 1 0 103.77 8.27 7 -1 0 99.91 8.14 7 -1 0 105.82 8.37 7 1 0 104.22 8.24 -7 1 0 102.17 8.60 -7 1 0 92.70 7.50 7 -1 0 94.86 7.84 -7 -1 0 116.94 9.53 7 1 0 96.41 7.84 -7 1 0 101.72 9.00 -7 -1 -1 17.36 3.50 -7 1 -1 15.07 3.24 7 1 1 18.17 3.52 7 -1 1 15.66 3.22 7 -1 1 14.66 3.13 7 1 1 24.55 4.01 -7 1 -1 20.33 3.95 -7 1 -1 15.38 3.02 7 1 1 15.70 3.14 -7 -1 -1 13.93 3.38 7 1 2 377.69 15.38 7 -1 2 393.31 15.65 -7 -1 -2 391.21 17.28 7 1 2 364.41 14.38 -7 1 -2 367.55 16.76 -7 1 -2 352.77 15.91 -7 1 -2 365.73 15.21 -7 -1 -2 363.15 15.37 7 1 2 376.64 15.23 7 -1 2 390.27 15.51 7 1 3 342.15 14.25 7 -1 3 331.53 14.06 -7 1 -3 305.48 13.59 -7 -1 -3 323.91 14.12 7 1 3 322.21 13.86 7 -1 3 335.60 13.93 -7 -1 -3 322.18 15.51 -7 1 -3 327.83 15.31 7 1 4 82.90 6.81 7 -1 4 78.80 6.70 7 -1 4 84.42 7.17 -7 1 -4 80.91 7.36 -7 1 -4 72.10 6.42 -7 -1 -4 72.13 6.46 7 1 4 78.38 6.68 7 -1 4 72.79 6.32 7 -1 5 336.74 12.40 7 1 5 332.32 13.14 7 -1 5 351.21 13.36 -7 1 -5 330.71 13.95 -7 1 -5 316.96 12.74 -7 -1 -5 321.93 13.01 7 -1 5 346.39 13.75 -7 -1 -5 340.75 14.80 7 1 5 330.47 11.88 -7 1 -5 341.10 14.10 7 1 5 346.02 13.48 7 -1 5 336.04 12.83 7 -1 6 1.59 1.19 7 1 6 -0.14 0.50 -7 -1 -6 1.20 1.19 -7 1 -6 2.30 1.17 7 1 6 1.79 1.03 7 -1 6 0.91 0.87 7 1 6 1.73 1.04 7 -1 6 0.96 0.87 7 -1 6 0.54 0.81 7 -1 7 140.97 7.32 -7 1 -7 139.44 7.23 7 1 7 148.17 7.55 7 -1 7 157.36 7.78 7 1 7 146.92 7.69 7 -1 7 140.82 7.08 7 -1 7 146.28 7.33 7 1 8 2.98 1.08 7 1 8 4.09 1.15 7 -1 8 3.07 1.03 7 -1 8 1.97 0.81 7 -1 8 1.26 0.68 7 1 8 4.41 1.20 7 2 -10 385.23 9.34 -7 -2 10 412.14 10.63 7 -2 -9 3.01 1.07 7 2 -9 3.85 1.03 7 2 -9 3.55 1.19 -7 -2 9 3.21 1.21 7 -2 -8 365.17 12.15 7 -2 -8 363.73 11.89 7 -2 -7 114.46 7.13 7 2 -7 97.80 6.28 -7 2 7 98.01 6.71 7 -2 -7 101.96 6.84 -7 2 7 88.35 6.38 -7 2 6 290.56 12.18 7 -2 -6 320.59 12.43 7 2 -6 308.51 11.80 7 -2 -6 325.39 12.14 -7 2 6 307.40 13.24 7 2 -6 268.75 9.57 7 -2 -6 336.39 12.96 7 2 -6 311.27 12.56 7 2 -5 64.45 5.96 -7 2 5 73.19 6.63 -7 -2 5 54.68 5.30 7 -2 -5 65.71 5.81 7 2 -5 67.62 5.80 7 -2 -5 73.23 6.02 -7 2 5 62.31 6.17 -7 2 5 52.04 5.34 7 2 -5 57.12 4.85 7 -2 -5 63.52 5.84 -7 2 5 64.30 5.95 -7 -2 4 233.40 10.80 7 -2 -4 234.50 11.16 7 2 -4 223.67 10.78 7 -2 -4 235.79 11.05 -7 2 4 234.79 12.10 -7 2 4 213.23 10.86 7 2 -4 232.10 10.17 7 -2 -4 240.89 11.56 7 2 -4 219.71 11.12 -7 2 4 234.22 12.43 -7 -2 3 115.80 7.49 7 2 -3 125.88 8.23 7 -2 -3 124.04 8.15 7 -2 -3 123.03 8.20 -7 2 3 109.13 7.83 7 2 -3 122.94 8.41 -7 2 3 126.35 9.41 7 -2 -3 122.53 8.31 7 2 -3 124.04 7.77 -7 2 3 109.59 8.29 7 2 -2 7.76 2.21 -7 2 2 1.52 1.29 -7 -2 2 2.48 1.21 -7 2 2 5.88 1.90 7 2 -2 3.26 1.38 7 -2 -2 1.70 1.15 7 2 -2 3.72 1.52 7 -2 -2 2.54 1.39 -7 2 2 1.51 1.14 7 2 -1 117.70 8.12 -7 -2 1 115.28 6.72 7 2 -1 117.71 8.05 7 -2 -1 124.47 8.32 -7 2 1 117.10 8.55 -7 2 1 107.58 7.67 7 -2 -1 117.59 8.15 7 2 -1 112.52 7.69 -7 2 1 107.70 8.05 -7 2 0 39.35 4.84 7 2 0 46.27 5.05 7 -2 0 42.36 4.91 -7 2 0 42.89 4.71 7 -2 0 50.65 5.31 7 2 0 42.56 4.78 7 2 0 40.31 4.67 -7 2 0 51.48 6.15 -7 2 0 44.39 5.38 -7 2 -1 0.94 0.94 -7 2 -1 4.14 1.85 7 2 1 2.02 1.30 7 -2 1 4.29 1.63 7 2 1 3.37 1.51 7 -2 1 4.95 1.75 7 2 1 3.38 1.49 -7 -2 -1 3.44 1.77 -7 2 -1 0.88 1.08 7 2 2 13.39 2.71 7 -2 2 15.80 2.89 -7 2 -2 10.00 2.36 -7 2 -2 12.68 2.92 7 2 2 14.06 2.82 7 -2 2 16.28 2.93 7 -2 2 21.89 3.75 7 2 2 14.88 2.64 -7 -2 -2 11.46 2.85 -7 2 -2 13.07 2.98 7 2 3 292.44 12.03 7 -2 3 306.19 11.93 7 2 3 286.57 11.79 7 -2 3 308.68 12.19 -7 2 -3 284.34 11.67 -7 2 -3 269.33 11.42 -7 -2 -3 334.31 14.82 -7 2 -3 297.92 13.47 7 2 4 407.76 13.42 7 2 4 404.50 13.69 -7 2 -4 389.57 14.52 -7 2 -4 427.35 15.50 7 2 5 11.46 2.14 -7 -2 -5 7.60 1.50 7 2 5 12.91 2.39 7 -2 5 11.82 2.53 -7 2 -5 10.66 2.31 -7 2 -5 9.47 2.28 7 2 6 223.60 8.48 7 2 6 257.79 9.68 7 -2 6 270.34 10.67 -7 2 -6 236.72 9.04 -7 2 -6 252.78 10.21 7 2 7 1.00 0.65 7 2 7 2.27 0.83 7 -2 7 2.57 0.98 -7 -2 -7 1.53 0.73 7 2 8 182.41 6.12 7 -2 8 216.71 6.91 7 3 -9 56.03 3.41 -7 -3 9 65.75 3.94 7 3 -8 71.06 4.52 -7 -3 8 74.41 4.87 7 3 -7 271.54 9.66 -7 -3 7 277.95 10.21 7 3 -6 339.10 11.45 -7 3 6 367.78 12.56 -7 3 6 362.64 12.66 -7 -3 6 369.08 12.37 7 3 -5 2.46 1.18 -7 3 5 3.39 1.46 -7 3 5 3.39 1.43 -7 -3 5 2.58 1.21 -7 3 4 86.37 6.30 7 3 -4 84.51 6.04 -7 3 4 95.17 7.21 -7 3 4 82.71 6.32 -7 -3 4 95.36 6.48 -7 3 3 25.70 3.54 -7 -3 3 24.86 3.30 7 3 -3 23.53 3.22 -7 3 3 22.30 3.31 -7 3 2 503.97 15.74 -7 -3 2 523.15 14.39 7 3 -2 455.18 11.95 -7 3 2 520.37 15.45 -7 3 2 473.01 15.02 7 3 -2 529.67 14.80 7 3 -1 0.67 0.87 -7 3 1 3.76 1.81 -7 3 1 2.10 1.14 -7 -3 1 1.35 0.87 7 3 -1 1.50 0.84 -7 3 1 0.20 0.59 -7 3 1 4.35 1.60 7 3 0 549.32 13.14 -7 3 0 600.95 16.56 -7 3 0 635.02 18.34 -7 -3 0 652.28 18.19 7 3 0 592.79 14.58 -7 3 0 682.72 19.82 -7 3 -1 83.56 6.64 -7 3 -1 86.33 6.89 -7 -3 -1 94.39 6.99 -7 -3 -2 383.66 13.88 7 -3 2 422.01 13.88 -7 3 -2 397.33 14.15 -7 -3 -3 113.19 6.71 7 -3 3 115.54 7.08 -7 3 -3 110.74 6.97 -7 -3 -4 254.50 10.32 -7 3 -4 238.54 9.56 -7 -3 -4 229.40 8.44 -7 3 -4 246.31 10.33 7 -3 4 266.82 10.40 -7 3 -4 257.35 9.52 -7 3 -5 4.80 1.29 -7 3 -5 3.04 1.14 7 -3 5 3.31 1.19 -7 -3 -5 1.17 0.82 -7 3 -6 4.87 1.19 -7 -3 -6 5.64 1.22 -7 3 -6 5.53 1.28 7 -3 6 6.36 1.40 -7 4 6 342.34 9.10 -7 -4 6 347.84 9.32 -7 4 5 128.91 5.95 -7 -4 5 134.43 6.22 -7 4 5 134.87 6.62 -7 4 4 26.10 2.74 -7 -4 4 25.16 2.77 -7 -4 3 333.99 10.57 -7 -4 3 342.59 10.07 -7 -4 2 55.73 4.56 -7 -4 2 46.51 3.62 -7 4 2 60.40 5.01 -7 -4 1 30.72 2.87 -7 4 1 46.96 4.35 -7 -4 0 54.74 4.37 -7 4 0 51.82 4.39 -7 -4 0 50.78 4.41 -7 4 0 44.01 4.06 -7 -4 -1 180.86 7.90 -7 4 -1 168.97 7.38 -7 -4 -1 172.84 7.82 -7 4 -1 163.54 7.67 -7 -4 -2 27.41 3.05 -7 -4 -2 29.36 3.04 -7 4 -2 22.23 2.41 -7 4 -2 25.57 2.82 -7 4 -3 130.89 5.98 -7 -4 -3 135.17 5.68 -7 4 -3 151.18 6.68 -7 -4 -4 148.34 5.91 -7 4 -4 142.63 5.69 0 0 0 0.00 0.00 TITL Z483101_g in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 6.142903 8.106683 17.960480 90.0000 93.2790 90.0000 ZERR 4.00 0.000035 0.000053 0.000085 0.0000 0.0005 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O Br UNIT 32.00 12.00 16.00 12.00 4.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 SIZE 0.17 0.23 0.27 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 18239 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Br8 Br 0.28778(3) 0.15736(2) 0.53190(2) 0.01687(9) Uani 1 1 d . . . . . O1 O 0.1003(2) 0.27894(18) 0.22864(8) 0.0170(3) Uani 1 1 d . . . . . O2 O 0.3081(2) 0.41895(17) 0.14573(7) 0.0166(3) Uani 1 1 d . . . . . O5 O 1.0181(2) 0.57228(18) 0.33823(8) 0.0193(3) Uani 1 1 d . . . . . N1 N 0.2686(3) 0.35672(19) 0.22017(9) 0.0140(3) Uani 1 1 d . . . . . N3 N 0.5086(3) 0.4965(2) 0.14844(9) 0.0170(3) Uani 1 1 d . . . . . N4 N 0.7821(3) 0.5491(2) 0.24253(9) 0.0162(3) Uani 1 1 d . . . . . N5 N 0.8383(3) 0.5186(2) 0.31208(9) 0.0150(3) Uani 1 1 d . . . . . C3A C 0.5843(3) 0.4841(2) 0.21833(10) 0.0144(4) Uani 1 1 d . . . . . C5A C 0.7080(3) 0.4268(2) 0.36301(10) 0.0138(4) Uani 1 1 d . . . . . C6 C 0.7951(3) 0.3973(2) 0.43497(11) 0.0159(4) Uani 1 1 d . . . . . H6 H 0.938642 0.432970 0.449517 0.019 Uiso 1 1 calc R U . . . C7 C 0.6705(3) 0.3155(3) 0.48518(11) 0.0172(4) Uani 1 1 d . . . . . H7 H 0.727913 0.294264 0.534483 0.021 Uiso 1 1 calc R U . . . C8 C 0.4595(3) 0.2644(2) 0.46272(10) 0.0149(4) Uani 1 1 d . . . . . C9 C 0.3726(3) 0.2891(2) 0.39083(10) 0.0139(4) Uani 1 1 d . . . . . H9 H 0.229869 0.251621 0.376337 0.017 Uiso 1 1 calc R U . . . C9A C 0.4988(3) 0.3701(2) 0.34009(10) 0.0129(3) Uani 1 1 d . . . . . C9B C 0.4407(3) 0.3999(2) 0.26317(10) 0.0129(3) 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 Br8 0.01888(13) 0.01734(13) 0.01471(12) 0.00324(7) 0.00369(7) 0.00016(7) O1 0.0143(6) 0.0159(7) 0.0205(7) -0.0005(5) -0.0011(5) -0.0026(5) O2 0.0190(7) 0.0173(7) 0.0133(6) 0.0015(5) -0.0005(5) 0.0011(5) O5 0.0136(6) 0.0188(7) 0.0254(7) -0.0002(6) -0.0005(5) -0.0052(5) N1 0.0173(8) 0.0117(7) 0.0131(7) 0.0007(6) 0.0003(6) 0.0026(6) N3 0.0176(8) 0.0164(8) 0.0171(8) 0.0020(6) 0.0022(6) 0.0024(6) N4 0.0166(8) 0.0142(8) 0.0181(8) 0.0020(6) 0.0036(6) 0.0010(6) N5 0.0138(7) 0.0122(8) 0.0190(8) -0.0009(6) 0.0023(6) 0.0001(6) C3A 0.0177(9) 0.0101(8) 0.0155(8) 0.0002(7) 0.0026(7) 0.0037(7) C5A 0.0149(8) 0.0111(8) 0.0156(8) -0.0007(7) 0.0028(7) -0.0001(7) C6 0.0149(8) 0.0148(9) 0.0179(9) -0.0024(7) -0.0014(7) -0.0011(7) C7 0.0195(9) 0.0172(9) 0.0146(8) 0.0001(7) -0.0014(7) 0.0015(8) C8 0.0174(9) 0.0106(8) 0.0170(9) 0.0011(7) 0.0045(7) 0.0000(7) C9 0.0138(8) 0.0116(9) 0.0163(8) -0.0009(7) 0.0016(7) 0.0004(7) C9A 0.0149(8) 0.0093(8) 0.0144(8) -0.0015(7) 0.0007(6) 0.0011(7) C9B 0.0131(8) 0.0097(8) 0.0158(8) -0.0006(7) 0.0010(6) 0.0013(7) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0819 0 0 1 0.0903 0 -1 1 0.1371 0 1 -1 0.1465 -1 -1 0 0.1157 1 1 0 0.1385 1 0 1 0.1084 -1 0 -1 0.1008 0 -1 0 0.1411 0 1 0 0.1300 -1 1 1 0.1319 1 -1 -1 0.1319 -1 -1 1 0.1075 1 0 -1 0.1200 -1 0 1 0.1092 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 N3 O2 N1 108.60(13) . . ? O1 N1 C9B 135.68(17) . . ? O1 N1 O2 118.38(15) . . ? C9B N1 O2 105.92(15) . . ? C3A N3 O2 105.32(15) . . ? N5 N4 C3A 114.37(15) . . ? O5 N5 N4 118.27(16) . . ? O5 N5 C5A 116.55(15) . . ? N4 N5 C5A 125.17(16) . . ? N3 C3A N4 122.03(17) . . ? N3 C3A C9B 112.61(17) . . ? N4 C3A C9B 125.36(17) . . ? C6 C5A C9A 120.91(17) . . ? C6 C5A N5 118.40(17) . . ? C9A C5A N5 120.69(16) . . ? C7 C6 C5A 119.29(18) . . ? C7 C6 H6 120.4 . . ? C5A C6 H6 120.4 . . ? C6 C7 C8 119.47(18) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 121.90(17) . . ? C9 C8 Br8 118.73(14) . . ? C7 C8 Br8 119.37(14) . . ? C8 C9 C9A 118.61(17) . . ? C8 C9 H9 120.7 . . ? C9A C9 H9 120.7 . . ? C9 C9A C5A 119.75(17) . . ? C9 C9A C9B 126.48(17) . . ? C5A C9A C9B 113.74(16) . . ? N1 C9B C3A 107.54(16) . . ? N1 C9B C9A 131.97(18) . . ? C3A C9B C9A 120.44(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 Br8 C8 1.8867(19) . ? O1 N1 1.228(2) . ? O2 N3 1.381(2) . ? O2 N1 1.462(2) . ? O5 N5 1.253(2) . ? N1 C9B 1.320(2) . ? N3 C3A 1.317(3) . ? N4 N5 1.301(2) . ? N4 C3A 1.372(3) . ? N5 C5A 1.455(2) . ? C3A C9B 1.405(3) . ? C5A C6 1.391(3) . ? C5A C9A 1.404(3) . ? C6 C7 1.385(3) . ? C6 H6 0.9500 . ? C7 C8 1.398(3) . ? C7 H7 0.9500 . ? C8 C9 1.383(3) . ? C9 C9A 1.394(3) . ? C9 H9 0.9500 . ? C9A C9B 1.427(3) . ? 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 N3 O2 N1 O1 -177.78(15) . . . . ? N3 O2 N1 C9B 0.67(18) . . . . ? N1 O2 N3 C3A -0.47(18) . . . . ? C3A N4 N5 O5 179.21(16) . . . . ? C3A N4 N5 C5A -1.1(3) . . . . ? O2 N3 C3A N4 -179.46(16) . . . . ? O2 N3 C3A C9B 0.1(2) . . . . ? N5 N4 C3A N3 -176.47(17) . . . . ? N5 N4 C3A C9B 4.0(3) . . . . ? O5 N5 C5A C6 -3.4(3) . . . . ? N4 N5 C5A C6 176.89(18) . . . . ? O5 N5 C5A C9A 176.25(17) . . . . ? N4 N5 C5A C9A -3.5(3) . . . . ? C9A C5A C6 C7 -2.0(3) . . . . ? N5 C5A C6 C7 177.60(17) . . . . ? C5A C6 C7 C8 -0.1(3) . . . . ? C6 C7 C8 C9 1.8(3) . . . . ? C6 C7 C8 Br8 -178.57(15) . . . . ? C7 C8 C9 C9A -1.2(3) . . . . ? Br8 C8 C9 C9A 179.16(14) . . . . ? C8 C9 C9A C5A -1.0(3) . . . . ? C8 C9 C9A C9B 176.97(18) . . . . ? C6 C5A C9A C9 2.6(3) . . . . ? N5 C5A C9A C9 -177.00(17) . . . . ? C6 C5A C9A C9B -175.58(17) . . . . ? N5 C5A C9A C9B 4.8(2) . . . . ? O1 N1 C9B C3A 177.5(2) . . . . ? O2 N1 C9B C3A -0.59(19) . . . . ? O1 N1 C9B C9A 0.2(4) . . . . ? O2 N1 C9B C9A -177.88(19) . . . . ? N3 C3A C9B N1 0.3(2) . . . . ? N4 C3A C9B N1 179.88(17) . . . . ? N3 C3A C9B C9A 178.00(17) . . . . ? N4 C3A C9B C9A -2.5(3) . . . . ? C9 C9A C9B N1 -3.2(3) . . . . ? C5A C9A C9B N1 174.89(19) . . . . ? C9 C9A C9B C3A 179.81(18) . . . . ? C5A C9A C9B C3A -2.1(3) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0002 -0.0000 -0.9996 -0.0248 -0.0781 -0.0257 -0.0002 0.0000 0.9996 0.0248 0.0781 0.0257 -0.0002 -0.9993 0.9998 0.0533 0.0114 0.2012 0.0002 0.9993 -0.9998 -0.0533 -0.0114 -0.2012 -0.9998 -0.9994 -0.0011 -0.2127 -0.0240 0.2308 0.9998 0.9994 0.0011 0.2127 0.0240 -0.2308 0.9997 0.0001 1.0009 0.2660 0.0354 -0.0296 -0.9997 -0.0001 -1.0009 -0.2660 -0.0354 0.0296 0.0000 -0.9993 0.0002 0.0285 -0.0667 0.1755 -0.0000 0.9993 -0.0002 -0.0285 0.0667 -0.1755 -1.0000 0.9993 0.9982 -0.2449 0.1875 -0.0946 1.0000 -0.9993 -0.9982 0.2449 -0.1875 0.0946 -1.0000 -0.9994 0.9985 -0.1879 0.0541 0.2565 1.0000 0.0000 -0.9983 0.2164 -0.1208 -0.0809 -1.0000 -0.0000 0.9983 -0.2164 0.1208 0.0809