#------------------------------------------------------------------------------ #$Date: 2019-11-23 09:00:35 +0200 (Sat, 23 Nov 2019) $ #$Revision: 232623 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/34/79/4347992.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_4347992 loop_ _publ_author_name 'Dolgopolova, Ekaterina A.' 'Rice, Allison M.' 'Smith, Mark D.' 'Shustova, Natalia B.' _publ_section_title ; Photophysics, Dynamics, and Energy Transfer in Rigid Mimics of GFP-based Systems. ; _journal_issue 15 _journal_name_full 'Inorganic chemistry' _journal_page_first 7257 _journal_page_last 7264 _journal_paper_doi 10.1021/acs.inorgchem.6b00835 _journal_volume 55 _journal_year 2016 _chemical_formula_moiety 'C12 H11 Br N2 O' _chemical_formula_sum 'C12 H11 Br N2 O' _chemical_formula_weight 279.14 _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 direct _audit_creation_date 2016-03-10 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _cell_angle_alpha 91.050(2) _cell_angle_beta 90.542(2) _cell_angle_gamma 117.540(2) _cell_formula_units_Z 4 _cell_length_a 7.5315(6) _cell_length_b 8.0931(7) _cell_length_c 20.7005(16) _cell_measurement_reflns_used 3042 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.069 _cell_measurement_theta_min 2.840 _cell_volume 1118.37(16) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEXII v2014.9-0 (Bruker, 2014)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker PHOTON-100 area detector' _diffrn_detector_area_resol_mean 10.4 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 5366 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 26.498 _diffrn_reflns_theta_max 26.498 _diffrn_reflns_theta_min 2.839 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _exptl_absorpt_coefficient_mu 3.654 _exptl_absorpt_correction_T_max 0.2602 _exptl_absorpt_correction_T_min 0.2127 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.0770 before and 0.0315 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.0717 before and 0.0309 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.658 _exptl_crystal_description plate _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.487 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 294 _refine_ls_number_reflns 5366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.995 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0357 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.0616 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4427 _reflns_number_total 5366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ic6b00835_si_008.cif _cod_data_source_block ead_2_3br _cod_database_code 4347992 _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 0.931 _shelx_estimated_absorpt_t_min 0.500 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.4952(6) 0.5048(6) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3.a Aromatic/amide H refined with riding coordinates: C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A), C12A(H12A), C6B(H6B), C8B(H8B), C9B(H9B), C10B(H10B), C12B(H12B) 3.b Idealised Me refined as rotating group: C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB, H5BC) ; _shelx_res_file ; ead_2_3br.res created by SHELXL-2014/7 TITL twin6 in P-1 #2 REM reset to P-1 #2 CELL 0.71073 7.5315 8.0931 20.7005 91.0501 90.5416 117.5397 ZERR 4 0.0006 0.0007 0.0016 0.0021 0.0021 0.002 LATT 1 SFAC C H Br N O UNIT 48 44 4 8 4 L.S. 7 PLAN 9 SIZE 0.02 0.16 0.22 TEMP -173(2) LIST 4 MORE -1 BOND $H CONF fmap 2 acta 53.0 REM REM REM WGHT 0.031900 BASF 0.50481 FVAR 0.55977 BR1A 3 0.043024 0.531624 0.233372 11.00000 0.01784 0.02801 = 0.01838 0.00072 0.00497 0.01293 O1A 5 0.658546 0.973032 -0.077121 11.00000 0.02190 0.01845 = 0.02049 0.00634 0.00322 0.01330 N1A 4 0.903880 0.874665 -0.083007 11.00000 0.01424 0.01324 = 0.01053 0.00325 0.00347 0.00754 N2A 4 0.839281 0.697503 0.005376 11.00000 0.01356 0.01005 = 0.01385 0.00108 0.00162 0.00706 C1A 1 0.740962 0.886262 -0.056228 11.00000 0.01341 0.01108 = 0.01279 -0.00358 0.00153 0.00229 C2A 1 0.701881 0.768656 0.001702 11.00000 0.01140 0.01225 = 0.01227 -0.00015 0.00041 0.00403 C3A 1 0.952248 0.762450 -0.044887 11.00000 0.01237 0.01093 = 0.01464 -0.00140 -0.00248 0.00390 C4A 1 1.123098 0.725877 -0.061354 11.00000 0.01314 0.01488 = 0.02201 0.00086 0.00269 0.00737 AFIX 137 H4AA 2 1.102288 0.670640 -0.105053 11.00000 -1.50000 H4AB 2 1.131590 0.639559 -0.030372 11.00000 -1.50000 H4AC 2 1.247883 0.843356 -0.059478 11.00000 -1.50000 AFIX 0 C5A 1 1.000926 0.969117 -0.141561 11.00000 0.02251 0.01527 = 0.01677 0.00676 0.00500 0.00720 AFIX 137 H5AA 2 0.922461 1.024042 -0.161394 11.00000 -1.50000 H5AB 2 1.009666 0.879112 -0.172005 11.00000 -1.50000 H5AC 2 1.135941 1.067743 -0.130677 11.00000 -1.50000 AFIX 0 C6A 1 0.551802 0.742656 0.042227 11.00000 0.01041 0.00855 = 0.01781 -0.00149 -0.00458 0.00668 AFIX 43 H6A 2 0.474057 0.802777 0.030612 11.00000 -1.20000 AFIX 0 C7A 1 0.492344 0.636545 0.100736 11.00000 0.00822 0.00955 = 0.01388 -0.00219 -0.00419 0.00143 C8A 1 0.585754 0.539217 0.126238 11.00000 0.01140 0.01354 = 0.02066 0.00046 0.00335 0.00629 AFIX 43 H8A 2 0.695493 0.538230 0.104298 11.00000 -1.20000 AFIX 0 C9A 1 0.522339 0.442980 0.183239 11.00000 0.01189 0.01765 = 0.01602 0.00302 -0.00056 0.00421 AFIX 43 H9A 2 0.588779 0.377133 0.199837 11.00000 -1.20000 AFIX 0 C10A 1 0.363728 0.442531 0.215798 11.00000 0.01458 0.01547 = 0.01327 0.00433 -0.00226 0.00683 AFIX 43 H10A 2 0.321458 0.379253 0.255321 11.00000 -1.20000 AFIX 0 C11A 1 0.266871 0.536515 0.189646 11.00000 0.00841 0.01204 = 0.01798 -0.00275 0.00499 0.00112 C12A 1 0.328464 0.634511 0.133586 11.00000 0.01400 0.01112 = 0.01607 -0.00142 -0.00008 0.00793 AFIX 43 H12A 2 0.261257 0.699971 0.117252 11.00000 -1.20000 AFIX 0 BR1B 3 0.974322 -0.110221 0.313134 11.00000 0.02441 0.02329 = 0.02381 0.00096 0.00503 0.01729 O1B 5 0.920983 0.700451 0.502857 11.00000 0.01688 0.01440 = 0.01959 -0.00190 -0.00401 0.00719 N1B 4 0.646865 0.730231 0.465153 11.00000 0.01243 0.01172 = 0.01438 -0.00105 0.00036 0.00610 N2B 4 0.518650 0.498801 0.388485 11.00000 0.01067 0.01477 = 0.01730 0.00088 0.00070 0.00683 C1B 1 0.775362 0.651170 0.467091 11.00000 0.01284 0.01153 = 0.01554 0.00895 0.00524 0.00657 C2B 1 0.688645 0.499643 0.417719 11.00000 0.01296 0.00926 = 0.00593 -0.00051 0.00117 0.00247 C3B 1 0.499044 0.634397 0.417954 11.00000 0.01182 0.01480 = 0.01782 0.00903 0.00568 0.00519 C4B 1 0.339363 0.687657 0.404317 11.00000 0.01649 0.02031 = 0.01414 0.00383 0.00161 0.00991 AFIX 137 H4BA 2 0.258568 0.669541 0.442893 11.00000 -1.50000 H4BB 2 0.253735 0.609747 0.368520 11.00000 -1.50000 H4BC 2 0.400022 0.818960 0.392507 11.00000 -1.50000 AFIX 0 C5B 1 0.671441 0.887061 0.506338 11.00000 0.01476 0.01515 = 0.02356 -0.00372 -0.00454 0.00699 AFIX 137 H5BA 2 0.753311 0.894896 0.544480 11.00000 -1.50000 H5BB 2 0.539757 0.869520 0.520005 11.00000 -1.50000 H5BC 2 0.737828 1.002518 0.482302 11.00000 -1.50000 AFIX 0 C6B 1 0.773686 0.387870 0.405969 11.00000 0.00894 0.01411 = 0.01211 0.00597 -0.00326 0.00136 AFIX 43 H6B 2 0.887785 0.413812 0.432425 11.00000 -1.20000 AFIX 0 C7B 1 0.719759 0.233561 0.359371 11.00000 0.01221 0.01401 = 0.01322 0.00344 0.00444 0.00667 C8B 1 0.557312 0.171498 0.315837 11.00000 0.01471 0.01706 = 0.01812 0.00008 -0.00060 0.01016 AFIX 43 H8B 2 0.469946 0.226522 0.316735 11.00000 -1.20000 AFIX 0 C9B 1 0.523711 0.027946 0.270886 11.00000 0.01348 0.01228 = 0.01465 0.00330 -0.00091 0.00281 AFIX 43 H9B 2 0.414454 -0.012456 0.240936 11.00000 -1.20000 AFIX 0 C10B 1 0.645479 -0.054226 0.269594 11.00000 0.01831 0.01303 = 0.02001 0.00026 0.00745 0.00562 AFIX 43 H10B 2 0.621773 -0.151638 0.239054 11.00000 -1.20000 AFIX 0 C11B 1 0.803864 0.005672 0.313197 11.00000 0.01425 0.01455 = 0.01183 0.00453 0.00744 0.00909 C12B 1 0.844335 0.147703 0.357948 11.00000 0.01167 0.01375 = 0.01316 0.00031 0.00026 0.00477 AFIX 43 H12B 2 0.954829 0.186705 0.387326 11.00000 -1.20000 AFIX 0 HKLF 5 REM twin6 in P-1 #2 REM R1 = 0.0357 for 4427 Fo > 4sig(Fo) and 0.0553 for all 5366 data REM 294 parameters refined using 0 restraints END WGHT 0.0319 0.0000 REM Highest difference peak 0.487, deepest hole -0.596, 1-sigma level 0.118 Q1 1 0.9048 -0.0878 0.3807 11.00000 0.05 0.49 Q2 1 0.1237 0.6688 0.2434 11.00000 0.05 0.49 Q3 1 1.0640 0.0187 0.3684 11.00000 0.05 0.46 Q4 1 0.5151 0.2997 0.2170 11.00000 0.05 0.45 Q5 1 0.6630 0.7814 0.0306 11.00000 0.05 0.44 Q6 1 0.1974 0.7361 0.3718 11.00000 0.05 0.44 Q7 1 0.5346 0.4052 0.4786 11.00000 0.05 0.42 Q8 1 0.7468 1.1138 -0.0990 11.00000 0.05 0.42 Q9 1 0.6412 0.1791 0.3482 11.00000 0.05 0.40 ; _shelx_res_checksum 71603 _shelx_hkl_file ; 1 0 0 469.457 3.54563 1 1 0 0 490.066 3.77809 2 1 0 0 894.622 13.6467 -2 1 0 0 894.622 13.6467 1 2 0 0 1542.13 11.1592 2 2 0 0 1475.19 10.7558 1 2 0 0 2404.71 49.0380 -2 2 0 0 2404.71 49.0380 1 3 0 0 1033.87 9.62674 1 3 0 0 2131.75 32.9677 -2 3 0 0 2131.75 32.9677 1 3 0 0 1069.69 10.0343 2 4 0 0 547.024 8.51917 2 4 0 0 540.544 8.50530 1 -5 0 1 4.80073 9.93755 -2 5 0 0 4.80073 9.93755 1 -6 0 1 161.932 12.3360 -2 6 0 0 161.932 12.3360 1 -7 0 1 3.97083 16.1643 -2 7 0 0 3.97083 16.1643 1 -8 0 1 3.19629 16.2607 -2 8 0 0 3.19629 16.2607 1 -8 1 1 96.8490 25.5988 -2 -8 1 0 96.8490 25.5988 1 -7 1 1 651.613 21.3207 -2 -7 1 0 651.613 21.3207 1 -6 1 1 735.855 17.3335 -2 -6 1 0 735.855 17.3335 1 -5 1 0 344.161 24.3205 -2 -5 1 0 344.161 24.3205 1 -5 1 0 173.458 9.13493 1 -5 1 0 184.036 9.34765 2 -4 1 0 38.5444 4.44462 2 -4 1 0 39.8944 4.41567 1 -4 1 0 71.3162 10.1493 -2 -4 1 0 71.3162 10.1493 1 -3 1 0 675.232 8.32212 -2 -3 1 0 675.232 8.32212 1 -2 1 0 0.47339 2.87715 -2 -2 1 0 0.47339 2.87715 1 -1 1 0 1070.39 8.27036 -2 -1 1 0 1070.39 8.27036 1 0 1 0 135.411 1.92138 1 0 1 0 280.154 4.33181 -2 0 1 0 280.154 4.33181 1 0 1 0 139.190 1.93527 2 1 1 0 12.6271 2.15321 1 1 1 0 10.7153 1.87308 2 1 1 0 28.2890 4.90813 -2 1 1 0 28.2890 4.90813 1 2 1 0 41.4524 3.16369 2 2 1 0 79.2022 8.90716 -2 2 1 0 79.2022 8.90716 1 2 1 0 39.9528 3.25918 1 3 1 0 3.10017 3.03388 2 3 1 0 3.69405 2.59505 1 -3 -1 1 800.573 39.6165 -2 3 1 0 800.573 39.6165 1 -4 -1 1 576.763 14.9664 -2 4 1 0 576.763 14.9664 1 4 1 0 128.485 8.35308 2 4 1 0 121.976 6.98568 1 -5 -1 1 723.011 13.2342 -2 5 1 0 723.011 13.2342 1 -6 -1 1 412.035 20.8738 -2 6 1 0 412.035 20.8738 1 -7 -1 1 269.116 24.9426 -2 7 1 0 269.116 24.9426 1 -9 2 1 89.7960 29.2605 -2 -9 2 0 89.7960 29.2605 1 -8 2 1 107.510 33.8461 -2 -8 2 0 107.510 33.8461 1 -7 2 1 68.8862 33.5419 -2 -7 2 0 68.8862 33.5419 1 -6 2 0 697.506 19.2839 -2 -6 2 0 697.506 19.2839 1 -6 2 0 339.223 28.8218 1 -6 2 0 345.148 28.8893 2 -5 2 0 1164.67 17.7846 -2 -5 2 0 1164.67 17.7846 1 -4 2 0 4149.34 31.9107 -2 -4 2 0 4149.34 31.9107 1 -3 2 0 1611.28 13.9907 -2 -3 2 0 1611.28 13.9907 1 -2 2 0 1593.56 12.4578 -2 -2 2 0 1593.56 12.4578 1 -1 2 0 755.615 8.48402 2 -1 2 0 1540.80 15.4771 -2 -1 2 0 1540.80 15.4771 1 -1 2 0 737.970 9.03639 1 0 2 0 1540.88 42.8235 -2 0 2 0 1540.88 42.8235 1 0 2 0 697.988 6.18460 1 0 2 0 727.878 6.15176 2 1 2 0 38.7799 2.34354 2 1 2 0 37.9742 2.04179 1 1 2 0 78.8419 17.2143 -2 1 2 0 78.8419 17.2143 1 2 2 0 207.172 6.44705 2 2 2 0 195.298 6.04418 1 -2 -2 1 221.590 15.0967 -2 2 2 0 221.590 15.0967 1 -3 -2 1 52.7461 8.41563 -2 3 2 0 52.7461 8.41563 1 -4 -2 1 81.4961 11.5778 -2 4 2 0 81.4961 11.5778 1 -5 -2 1 23.9380 12.2016 -2 5 2 0 23.9380 12.2016 1 -6 -2 1 40.8033 14.1732 -2 6 2 0 40.8033 14.1732 1 -7 -2 1 163.219 26.1297 -2 7 2 0 163.219 26.1297 1 -9 3 1 156.440 32.5958 -2 -9 3 0 156.440 32.5958 1 -7 3 0 197.109 51.5761 -2 -7 3 0 197.109 51.5761 1 -6 3 0 83.8133 15.4058 -2 -6 3 0 83.8133 15.4058 1 -5 3 0 223.459 10.8089 -2 -5 3 0 223.459 10.8089 1 -4 3 0 222.268 6.37218 -2 -4 3 0 222.268 6.37218 1 -3 3 0 979.617 8.75070 -2 -3 3 0 979.617 8.75070 1 -2 3 0 2208.34 17.6585 -2 -2 3 0 2208.34 17.6585 1 -1 3 0 756.433 11.3964 -2 -1 3 0 756.433 11.3964 1 -1 3 0 377.946 6.04335 2 -1 3 0 361.277 5.93245 1 0 3 0 272.080 4.16670 2 0 3 0 259.029 4.22234 1 0 3 0 576.229 14.7117 -2 0 3 0 576.229 14.7117 1 1 3 0 382.904 5.59900 2 1 3 0 377.504 5.65840 1 -1 -3 1 1108.89 23.9454 -2 1 3 0 1108.89 23.9454 1 -2 -3 1 809.099 11.8192 -2 2 3 0 809.099 11.8192 1 -3 -3 1 445.423 13.7610 -2 3 3 0 445.423 13.7610 1 -4 -3 1 281.676 13.4883 -2 4 3 0 281.676 13.4883 1 -5 -3 1 35.0083 18.1266 -2 5 3 0 35.0083 18.1266 1 -6 -3 1 29.7464 24.6060 -2 6 3 0 29.7464 24.6060 1 -9 4 1 405.301 93.1528 -2 -9 4 0 405.301 93.1528 1 -7 4 0 140.470 32.6255 -2 -7 4 0 140.470 32.6255 1 -6 4 0 140.836 14.0123 -2 -6 4 0 140.836 14.0123 1 -5 4 0 130.900 8.79398 -2 -5 4 0 130.900 8.79398 1 -4 4 0 48.1613 5.79774 -2 -4 4 0 48.1613 5.79774 1 -3 4 0 327.038 6.14372 -2 -3 4 0 327.038 6.14372 1 -2 4 0 237.076 6.81178 -2 -2 4 0 237.076 6.81178 1 -2 4 0 125.109 5.63171 2 -2 4 0 113.830 5.27726 1 -1 4 0 25.6848 2.87129 2 -1 4 0 20.3696 2.77389 1 -1 4 0 42.6722 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-1 5 20 15.5888 40.2785 1 0 -5 21 50.8897 34.4050 -2 0 5 20 50.8897 34.4050 1 4 -6 20 8.51971 50.3878 -2 -4 6 20 8.51971 50.3878 1 3 -6 20 12.0555 107.046 -2 3 -6 21 12.0555 107.046 -2 -3 6 20 12.0555 107.046 1 2 -6 21 42.6617 39.7316 -2 -2 6 20 42.6617 39.7316 1 -2 6 20 153.339 76.5495 -2 2 -6 21 153.339 76.5495 1 3 -6 21 62.8514 41.0114 2 0 5 20 61.1419 43.6254 -2 0 -5 21 61.1419 43.6254 1 -1 5 20 -74.456 50.5522 -2 1 -5 21 -74.456 50.5522 1 -3 5 21 15.5325 61.7955 -2 3 -5 21 15.5325 61.7955 1 -4 5 21 -17.679 35.2268 -2 4 -5 21 -17.679 35.2268 1 2 4 20 -7.4648 29.8454 -2 -2 -4 21 -7.4648 29.8454 1 1 4 20 95.5199 37.7987 -2 -1 -4 21 95.5199 37.7987 1 0 4 20 294.818 81.9001 -2 0 -4 21 294.818 81.9001 1 -2 4 21 274.919 36.1435 -2 2 -4 21 274.919 36.1435 1 -3 4 21 248.842 32.0879 -2 3 -4 21 248.842 32.0879 1 -4 4 21 177.131 24.0590 -2 4 -4 21 177.131 24.0590 1 -5 4 21 96.7180 25.0326 -2 5 -4 21 96.7180 25.0326 1 3 3 20 130.203 30.4493 -2 -3 -3 21 130.203 30.4493 1 2 3 20 117.445 36.6817 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17.4122 -2 0 -1 21 651.901 17.4122 1 -1 1 21 123.730 11.1252 -2 1 -1 21 123.730 11.1252 1 -2 1 21 325.377 22.9618 -2 2 -1 21 325.377 22.9618 1 -3 1 21 290.034 26.3239 -2 3 -1 21 290.034 26.3239 1 -4 1 21 223.033 42.2236 -2 4 -1 21 223.033 42.2236 1 5 0 20 76.4971 34.7237 -2 -5 0 21 76.4971 34.7237 1 4 0 20 175.894 75.0003 -2 -4 0 21 175.894 75.0003 1 3 0 21 91.4905 31.1438 -2 -3 0 21 91.4905 31.1438 1 2 0 21 63.0703 23.7777 -2 -2 0 21 63.0703 23.7777 1 1 0 21 16.4814 16.9943 -2 -1 0 21 16.4814 16.9943 1 0 0 21 7.24082 10.3368 -2 0 0 21 7.24082 10.3368 1 -1 0 21 5.00512 23.8243 -2 1 0 21 5.00512 23.8243 1 -2 0 21 87.4719 33.6333 -2 2 0 21 87.4719 33.6333 1 -3 0 21 36.4829 36.8425 -2 3 0 21 36.4829 36.8425 1 -4 0 21 29.0758 76.6383 -2 4 0 21 29.0758 76.6383 1 5 -1 21 179.853 65.6232 -2 -5 1 21 179.853 65.6232 1 5 -1 20 25.0561 106.228 -2 5 -1 21 25.0561 106.228 -2 -5 1 21 25.0561 106.228 1 4 -1 21 332.619 30.0152 -2 -4 1 21 332.619 30.0152 1 3 -1 21 252.850 25.8744 -2 -3 1 21 252.850 25.8744 1 2 -1 21 370.463 24.5709 -2 -2 1 21 370.463 24.5709 1 1 -1 21 122.667 11.3519 -2 -1 1 21 122.667 11.3519 1 0 -1 21 649.775 16.9347 -2 0 1 21 649.775 16.9347 1 -1 -1 21 361.439 22.5195 -2 1 1 21 361.439 22.5195 1 -2 -1 21 261.529 47.4601 -2 2 1 21 261.529 47.4601 1 -4 -1 22 72.8430 45.6203 -2 4 1 21 72.8430 45.6203 1 5 -2 21 104.144 32.4821 -2 -5 2 21 104.144 32.4821 1 4 -2 21 83.5460 27.0553 -2 -4 2 21 83.5460 27.0553 1 3 -2 21 101.876 23.5018 -2 -3 2 21 101.876 23.5018 1 2 -2 21 27.0652 14.1083 -2 -2 2 21 27.0652 14.1083 1 1 -2 21 86.5307 17.5801 -2 -1 2 21 86.5307 17.5801 1 0 -2 21 43.7545 18.8956 -2 0 2 21 43.7545 18.8956 1 -1 -2 21 147.413 47.1530 -2 1 2 21 147.413 47.1530 1 -2 -2 22 258.164 84.2895 -2 2 2 21 258.164 84.2895 1 -2 -2 21 73.2150 66.1153 -2 2 2 21 73.2150 66.1153 1 -3 -2 22 67.9380 43.7269 -2 3 2 21 67.9380 43.7269 1 5 -3 21 7.30399 29.1443 -2 -5 3 21 7.30399 29.1443 1 4 -3 21 282.816 27.7708 -2 -4 3 21 282.816 27.7708 1 3 -3 21 245.485 28.2225 -2 -3 3 21 245.485 28.2225 1 2 -3 21 -1.6172 18.7437 -2 -2 3 21 -1.6172 18.7437 1 1 -3 21 201.099 23.1544 -2 -1 3 21 201.099 23.1544 1 0 -3 21 86.3804 46.9253 -2 0 3 21 86.3804 46.9253 1 -1 -3 22 61.5032 50.1655 -2 1 3 21 61.5032 50.1655 1 -2 -3 22 38.6927 36.5460 -2 2 3 21 38.6927 36.5460 1 5 -4 21 115.641 29.1120 -2 -5 4 21 115.641 29.1120 1 4 -4 21 155.216 33.7217 -2 -4 4 21 155.216 33.7217 1 3 -4 21 233.110 34.3506 -2 -3 4 21 233.110 34.3506 1 2 -4 21 268.491 28.8375 -2 -2 4 21 268.491 28.8375 1 0 -4 22 127.026 54.2967 -2 0 4 21 127.026 54.2967 1 -1 -4 22 123.557 35.6489 -2 1 4 21 123.557 35.6489 1 4 -5 21 53.3672 39.3815 -2 -4 5 21 53.3672 39.3815 1 3 -5 21 96.8888 39.7072 -2 -3 5 21 96.8888 39.7072 1 1 -5 22 206.121 44.6461 -2 -1 5 21 206.121 44.6461 1 0 5 21 35.9274 19.9068 1 0 5 21 26.9471 24.0807 2 -1 5 21 196.995 53.6661 -2 1 -5 22 196.995 53.6661 1 -3 5 22 317.370 67.9395 -2 3 -5 22 317.370 67.9395 1 1 4 21 196.451 45.3322 -2 -1 -4 22 196.451 45.3322 1 0 4 21 84.9960 88.1738 -2 0 -4 22 84.9960 88.1738 1 -2 4 22 103.824 41.4715 -2 2 -4 22 103.824 41.4715 1 -3 4 22 75.4358 33.1917 -2 3 -4 22 75.4358 33.1917 1 -4 4 22 16.3211 32.0964 -2 4 -4 22 16.3211 32.0964 1 2 3 21 58.3378 42.8349 -2 -2 -3 22 58.3378 42.8349 1 -1 3 22 290.364 29.0474 -2 1 -3 22 290.364 29.0474 1 -2 3 22 114.254 32.5223 -2 2 -3 22 114.254 32.5223 1 -3 3 22 280.174 29.1154 -2 3 -3 22 280.174 29.1154 1 -4 3 22 103.379 24.1776 -2 4 -3 22 103.379 24.1776 1 3 2 21 126.851 33.6617 -2 -3 -2 22 126.851 33.6617 1 2 2 21 274.135 68.1752 -2 -2 -2 22 274.135 68.1752 1 1 2 22 212.547 57.8652 -2 -1 -2 22 212.547 57.8652 1 0 2 22 224.706 23.1006 -2 0 -2 22 224.706 23.1006 1 -1 2 22 216.576 19.1602 -2 1 -2 22 216.576 19.1602 1 -2 2 22 71.4394 21.6713 -2 2 -2 22 71.4394 21.6713 1 -3 2 22 76.7619 28.9780 -2 3 -2 22 76.7619 28.9780 1 -4 2 22 228.502 33.2545 -2 4 -2 22 228.502 33.2545 1 4 1 21 57.2451 33.1813 -2 -4 -1 22 57.2451 33.1813 1 3 1 21 127.299 75.4830 -2 -3 -1 22 127.299 75.4830 1 2 1 22 6.98644 45.9302 -2 -2 -1 22 6.98644 45.9302 1 1 1 22 26.8456 26.7938 -2 -1 -1 22 26.8456 26.7938 1 0 1 22 10.1481 20.8534 -2 0 -1 22 10.1481 20.8534 1 -1 1 22 16.5277 13.2278 -2 1 -1 22 16.5277 13.2278 1 -2 1 22 72.2575 22.4879 -2 2 -1 22 72.2575 22.4879 1 -3 1 22 73.8505 27.9372 -2 3 -1 22 73.8505 27.9372 1 -4 1 22 89.9937 44.5218 -2 4 -1 22 89.9937 44.5218 1 4 0 21 133.035 58.6271 -2 -4 0 22 133.035 58.6271 1 4 0 22 26.9069 83.9421 -2 -4 0 22 26.9069 83.9421 1 3 0 22 312.779 32.8308 -2 -3 0 22 312.779 32.8308 1 2 0 22 299.137 30.9373 -2 -2 0 22 299.137 30.9373 1 1 0 22 256.089 20.1919 -2 -1 0 22 256.089 20.1919 1 0 0 22 1315.70 22.0037 -2 0 0 22 1315.70 22.0037 1 -1 0 22 256.085 20.1919 -2 1 0 22 256.085 20.1919 1 -2 0 22 305.830 26.2045 -2 2 0 22 305.830 26.2045 1 -3 0 22 347.349 52.5464 -2 3 0 22 347.349 52.5464 1 -4 0 22 109.178 83.1049 -2 4 0 22 109.178 83.1049 1 -4 0 22 112.083 102.070 -2 -4 0 23 112.083 102.070 -2 4 0 22 112.083 102.070 1 4 0 22 14.0546 38.1636 2 4 -1 22 15.6143 33.9852 -2 -4 1 22 15.6143 33.9852 1 -4 1 22 42.5574 36.4101 1 3 -1 22 147.831 28.8462 -2 -3 1 22 147.831 28.8462 1 2 -1 22 100.521 19.6258 -2 -2 1 22 100.521 19.6258 1 1 -1 22 3.51943 13.3058 -2 -1 1 22 3.51943 13.3058 1 0 -1 22 31.1854 17.3762 -2 0 1 22 31.1854 17.3762 1 -1 -1 22 74.0064 48.8481 -2 1 1 22 74.0064 48.8481 1 -2 -1 22 -15.557 51.2374 -2 2 1 22 -15.557 51.2374 1 -5 2 22 133.841 18.5327 1 -5 2 22 107.327 41.1738 2 4 -2 22 290.770 30.6249 -2 -4 2 22 290.770 30.6249 1 3 -2 22 87.6297 21.9867 -2 -3 2 22 87.6297 21.9867 1 2 -2 22 55.0954 17.8334 -2 -2 2 22 55.0954 17.8334 1 1 -2 22 204.729 21.1847 -2 -1 2 22 204.729 21.1847 1 0 -2 22 164.216 30.1689 -2 0 2 22 164.216 30.1689 1 -1 -2 22 232.694 49.7903 -2 1 2 22 232.694 49.7903 1 -2 -2 22 236.790 73.8843 -2 2 2 22 236.790 73.8843 1 -2 -2 23 104.580 90.5520 -2 2 2 22 104.580 90.5520 1 3 2 22 34.6671 18.4100 2 3 2 22 44.2344 25.3763 1 -5 3 22 176.988 21.9053 2 -5 3 22 209.001 26.4097 1 4 -3 22 167.320 28.2929 -2 -4 3 22 167.320 28.2929 1 3 -3 22 258.487 25.0217 -2 -3 3 22 258.487 25.0217 1 2 -3 22 99.3596 23.3182 -2 -2 3 22 99.3596 23.3182 1 1 -3 22 177.382 33.0588 -2 -1 3 22 177.382 33.0588 1 0 -3 22 65.2070 52.6173 -2 0 3 22 65.2070 52.6173 1 -1 -3 22 92.9545 74.9215 -2 1 3 22 92.9545 74.9215 1 -1 -3 23 104.126 56.6121 -2 1 3 22 104.126 56.6121 1 2 3 22 11.5502 20.4932 1 2 3 22 9.48590 20.6995 2 4 -4 22 -0.3941 33.9401 -2 -4 4 22 -0.3941 33.9401 1 3 -4 22 51.6624 34.3573 -2 -3 4 22 51.6624 34.3573 1 2 -4 22 -6.3068 39.0396 -2 -2 4 22 -6.3068 39.0396 1 1 -4 22 -3.0245 73.6682 -2 -1 4 22 -3.0245 73.6682 1 0 -4 23 69.8379 56.8151 -2 0 4 22 69.8379 56.8151 1 0 -4 22 -20.864 99.9851 -2 0 -4 23 -20.864 99.9851 -2 0 4 22 -20.864 99.9851 1 3 -5 22 255.646 39.2520 -2 -3 5 22 255.646 39.2520 1 2 -5 22 219.770 75.4802 -2 -2 5 22 219.770 75.4802 1 0 4 22 11.8878 92.2577 -2 0 -4 23 11.8878 92.2577 1 -2 4 23 75.2540 41.0499 -2 2 -4 23 75.2540 41.0499 1 -3 4 23 215.831 36.5638 -2 3 -4 23 215.831 36.5638 1 0 3 23 224.671 91.8245 -2 0 -3 23 224.671 91.8245 1 -1 3 23 146.565 42.8175 -2 1 -3 23 146.565 42.8175 1 -2 3 23 153.254 30.6367 -2 2 -3 23 153.254 30.6367 1 -3 3 23 351.661 25.2718 -2 3 -3 23 351.661 25.2718 1 -4 3 23 66.3286 26.6800 -2 4 -3 23 66.3286 26.6800 1 0 2 23 61.1919 30.2795 -2 0 -2 23 61.1919 30.2795 1 -1 2 23 205.224 34.8872 -2 1 -2 23 205.224 34.8872 1 -2 2 23 130.678 22.7925 -2 2 -2 23 130.678 22.7925 1 -3 2 23 75.5276 27.8669 -2 3 -2 23 75.5276 27.8669 1 -4 2 23 142.351 32.9223 -2 4 -2 23 142.351 32.9223 1 3 1 23 156.959 104.237 -2 3 1 22 156.959 104.237 -2 -3 -1 23 156.959 104.237 1 3 1 23 218.761 89.6732 -2 -3 -1 23 218.761 89.6732 1 2 1 23 175.699 46.2095 -2 -2 -1 23 175.699 46.2095 1 1 1 23 364.359 27.7275 -2 -1 -1 23 364.359 27.7275 1 0 1 23 133.618 24.4188 -2 0 -1 23 133.618 24.4188 1 -1 1 23 273.288 17.3986 -2 1 -1 23 273.288 17.3986 1 -2 1 23 123.320 24.4253 -2 2 -1 23 123.320 24.4253 1 -3 1 23 90.7745 28.0295 -2 3 -1 23 90.7745 28.0295 1 -4 1 23 137.778 49.3778 -2 4 -1 23 137.778 49.3778 1 4 0 22 -47.419 92.1210 -2 -4 0 23 -47.419 92.1210 1 -4 0 23 8.43042 44.5035 1 3 0 23 32.9127 39.9534 -2 -3 0 23 32.9127 39.9534 1 2 0 23 -9.8876 31.6704 -2 -2 0 23 -9.8876 31.6704 1 1 0 23 41.3280 21.3578 -2 -1 0 23 41.3280 21.3578 1 0 0 23 9.26398 13.1258 -2 0 0 23 9.26398 13.1258 1 -1 0 23 65.9390 23.2601 -2 1 0 23 65.9390 23.2601 1 -2 0 23 15.4741 27.8362 -2 2 0 23 15.4741 27.8362 1 -3 0 23 27.4444 54.3014 -2 3 0 23 27.4444 54.3014 1 4 -1 23 47.6721 42.8246 -2 -4 1 23 47.6721 42.8246 1 4 -1 22 313.289 115.006 -2 4 -1 23 313.289 115.006 -2 -4 1 23 313.289 115.006 1 3 -1 23 154.307 29.2001 -2 -3 1 23 154.307 29.2001 1 2 -1 23 140.931 25.7141 -2 -2 1 23 140.931 25.7141 1 1 -1 23 256.131 19.5887 -2 -1 1 23 256.131 19.5887 1 0 -1 23 119.288 19.9067 -2 0 1 23 119.288 19.9067 1 -1 -1 23 329.779 24.0359 -2 1 1 23 329.779 24.0359 1 -2 -1 23 66.6996 54.5921 -2 2 1 23 66.6996 54.5921 1 -3 -1 23 245.353 88.5477 -2 3 1 23 245.353 88.5477 1 4 -2 23 96.5505 32.2446 -2 -4 2 23 96.5505 32.2446 1 3 -2 23 63.3208 25.1649 -2 -3 2 23 63.3208 25.1649 1 2 -2 23 166.045 27.0301 -2 -2 2 23 166.045 27.0301 1 1 -2 23 116.071 30.8351 -2 -1 2 23 116.071 30.8351 1 0 -2 23 79.7332 27.5061 -2 0 2 23 79.7332 27.5061 1 -1 -2 23 100.840 52.0604 -2 1 2 23 100.840 52.0604 1 -2 -2 23 19.1507 102.705 -2 -2 -2 24 19.1507 102.705 -2 2 2 23 19.1507 102.705 1 4 -3 23 78.0807 31.1543 -2 -4 3 23 78.0807 31.1543 1 3 -3 23 320.028 32.5188 -2 -3 3 23 320.028 32.5188 1 2 -3 23 61.9179 41.8176 -2 -2 3 23 61.9179 41.8176 1 1 -3 23 87.0649 37.4688 -2 -1 3 23 87.0649 37.4688 1 0 -3 23 125.547 83.5051 -2 0 3 23 125.547 83.5051 1 1 3 23 124.902 27.8433 1 -1 -3 23 267.151 100.864 -2 -1 -3 24 267.151 100.864 -2 1 3 23 267.151 100.864 1 3 -4 23 168.150 38.1560 -2 -3 4 23 168.150 38.1560 1 2 -4 23 51.8597 49.6411 -2 -2 4 23 51.8597 49.6411 1 1 -4 23 171.126 47.4242 -2 -1 4 23 171.126 47.4242 1 2 -4 24 -27.078 33.7257 1 2 -4 24 -10.363 40.9036 2 0 3 24 149.979 57.9529 -2 0 -3 24 149.979 57.9529 1 -1 3 24 164.212 49.9195 -2 1 -3 24 164.212 49.9195 1 -2 3 24 99.0583 40.4341 -2 2 -3 24 99.0583 40.4341 1 -3 3 24 32.9832 31.5722 -2 3 -3 24 32.9832 31.5722 1 2 2 23 160.874 86.2622 -2 -2 -2 24 160.874 86.2622 1 0 2 24 232.042 32.1365 -2 0 -2 24 232.042 32.1365 1 -1 2 24 196.702 29.9385 -2 1 -2 24 196.702 29.9385 1 -2 2 24 260.572 24.7196 -2 2 -2 24 260.572 24.7196 1 -3 2 24 99.4652 25.5855 -2 3 -2 24 99.4652 25.5855 1 2 1 24 199.460 49.6910 -2 -2 -1 24 199.460 49.6910 1 1 1 24 15.9710 30.8889 -2 -1 -1 24 15.9710 30.8889 1 0 1 24 7.66530 28.4989 -2 0 -1 24 7.66530 28.4989 1 -1 1 24 74.7744 18.1597 -2 1 -1 24 74.7744 18.1597 1 -2 1 24 20.8338 23.5878 -2 2 -1 24 20.8338 23.5878 1 -3 1 24 21.7115 28.2788 -2 3 -1 24 21.7115 28.2788 1 -3 0 24 129.943 30.1623 1 -3 0 24 79.6620 28.4773 2 3 0 24 97.4592 58.9591 -2 -3 0 24 97.4592 58.9591 1 2 0 24 316.712 34.9046 -2 -2 0 24 316.712 34.9046 1 1 0 24 309.828 27.2443 -2 -1 0 24 309.828 27.2443 1 0 0 24 335.059 26.8792 -2 0 0 24 335.059 26.8792 1 -1 0 24 288.672 29.8320 -2 1 0 24 288.672 29.8320 1 -2 0 24 301.273 28.2016 -2 2 0 24 301.273 28.2016 1 3 -1 24 31.9446 31.9628 -2 -3 1 24 31.9446 31.9628 1 2 -1 24 -41.413 35.9044 -2 -2 1 24 -41.413 35.9044 1 1 -1 24 56.4471 25.2822 -2 -1 1 24 56.4471 25.2822 1 0 -1 24 26.8829 24.0676 -2 0 1 24 26.8829 24.0676 1 -1 -1 24 39.4266 26.9274 -2 1 1 24 39.4266 26.9274 1 -2 -1 24 49.4361 60.3260 -2 2 1 24 49.4361 60.3260 1 3 -2 24 106.521 27.8425 -2 -3 2 24 106.521 27.8425 1 2 -2 24 218.591 35.3088 -2 -2 2 24 218.591 35.3088 1 1 -2 24 142.179 30.4011 -2 -1 2 24 142.179 30.4011 1 0 -2 24 213.135 32.9883 -2 0 2 24 213.135 32.9883 1 -1 -2 24 52.0716 44.9646 -2 1 2 24 52.0716 44.9646 1 3 -3 24 45.4736 33.1702 -2 -3 3 24 45.4736 33.1702 1 1 -3 24 89.9155 41.6428 -2 -1 3 24 89.9155 41.6428 1 0 -3 24 173.235 91.1588 -2 0 3 24 173.235 91.1588 1 0 2 25 -12.772 45.9432 -2 0 -2 25 -12.772 45.9432 1 -1 2 25 116.372 33.1245 -2 1 -2 25 116.372 33.1245 1 -2 2 25 72.9092 29.2009 -2 2 -2 25 72.9092 29.2009 1 1 1 25 241.249 35.1788 -2 -1 -1 25 241.249 35.1788 1 0 1 25 24.4367 31.7633 -2 0 -1 25 24.4367 31.7633 1 -1 1 25 69.3386 23.9387 -2 1 -1 25 69.3386 23.9387 1 -2 1 25 -8.5813 26.2825 -2 2 -1 25 -8.5813 26.2825 1 2 0 25 41.8830 34.8957 -2 -2 0 25 41.8830 34.8957 1 -2 0 25 9.67536 37.5843 1 -2 0 25 36.5766 38.6638 2 1 0 25 159.855 32.9313 -2 -1 0 25 159.855 32.9313 1 0 0 25 118.329 24.3769 -2 0 0 25 118.329 24.3769 1 -1 0 25 140.499 28.7804 -2 1 0 25 140.499 28.7804 1 -2 0 25 61.3422 33.2515 -2 2 0 25 61.3422 33.2515 1 2 -1 25 -32.215 33.8278 -2 -2 1 25 -32.215 33.8278 1 1 -1 25 27.5000 27.4243 -2 -1 1 25 27.5000 27.4243 1 0 -1 25 53.6480 31.1841 -2 0 1 25 53.6480 31.1841 1 -1 -1 25 193.972 31.7831 -2 1 1 25 193.972 31.7831 1 2 -2 25 169.466 31.7648 -2 -2 2 25 169.466 31.7648 1 1 -2 25 118.070 43.0279 -2 -1 2 25 118.070 43.0279 1 0 -2 25 20.0601 40.5098 -2 0 2 25 20.0601 40.5098 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 79370 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn Br1A Br 0.04302(6) 0.53162(5) 0.23337(2) 0.02046(12) Uani 1 1 d . O1A O 0.6585(4) 0.9730(3) -0.07712(13) 0.0186(7) Uani 1 1 d . N1A N 0.9039(4) 0.8747(4) -0.08301(15) 0.0121(8) Uani 1 1 d . N2A N 0.8393(4) 0.6975(4) 0.00538(16) 0.0118(7) Uani 1 1 d . C1A C 0.7410(6) 0.8863(5) -0.0562(2) 0.0138(10) Uani 1 1 d . C2A C 0.7019(5) 0.7687(4) 0.0017(2) 0.0125(9) Uani 1 1 d . C3A C 0.9522(5) 0.7624(5) -0.04489(19) 0.0133(9) Uani 1 1 d . C4A C 1.1231(5) 0.7259(5) -0.0614(2) 0.0163(10) Uani 1 1 d . H4AA H 1.1023 0.6706 -0.1051 0.024 Uiso 1 1 calc GR H4AB H 1.1316 0.6396 -0.0304 0.024 Uiso 1 1 calc GR H4AC H 1.2479 0.8434 -0.0595 0.024 Uiso 1 1 calc GR C5A C 1.0009(5) 0.9691(5) -0.14156(19) 0.0187(10) Uani 1 1 d . H5AA H 0.9225 1.0240 -0.1614 0.028 Uiso 1 1 calc GR H5AB H 1.0097 0.8791 -0.1720 0.028 Uiso 1 1 calc GR H5AC H 1.1359 1.0677 -0.1307 0.028 Uiso 1 1 calc GR C6A C 0.5518(5) 0.7427(4) 0.04223(18) 0.0114(9) Uani 1 1 d . H6A H 0.4741 0.8028 0.0306 0.014 Uiso 1 1 calc R C7A C 0.4923(5) 0.6365(5) 0.10074(19) 0.0117(9) Uani 1 1 d . C8A C 0.5858(5) 0.5392(4) 0.12624(19) 0.0150(10) Uani 1 1 d . H8A H 0.6955 0.5382 0.1043 0.018 Uiso 1 1 calc R C9A C 0.5223(5) 0.4430(5) 0.18324(19) 0.0162(10) Uani 1 1 d . H9A H 0.5888 0.3771 0.1998 0.019 Uiso 1 1 calc R C10A C 0.3637(5) 0.4425(5) 0.21580(19) 0.0144(9) Uani 1 1 d . H10A H 0.3215 0.3793 0.2553 0.017 Uiso 1 1 calc R C11A C 0.2669(5) 0.5365(5) 0.1896(2) 0.0142(9) Uani 1 1 d . C12A C 0.3285(5) 0.6345(5) 0.13359(19) 0.0129(9) Uani 1 1 d . H12A H 0.2613 0.7000 0.1173 0.016 Uiso 1 1 calc R Br1B Br 0.97432(6) -0.11022(5) 0.31313(2) 0.02135(13) Uani 1 1 d . O1B O 0.9210(4) 0.7005(3) 0.50286(14) 0.0170(6) Uani 1 1 d . N1B N 0.6469(4) 0.7302(4) 0.46515(15) 0.0127(8) Uani 1 1 d . N2B N 0.5187(4) 0.4988(4) 0.38849(15) 0.0139(8) Uani 1 1 d . C1B C 0.7754(6) 0.6512(5) 0.46709(19) 0.0128(9) Uani 1 1 d . C2B C 0.6886(6) 0.4996(5) 0.41772(19) 0.0104(9) Uani 1 1 d . C3B C 0.4990(6) 0.6344(5) 0.4180(2) 0.0150(10) Uani 1 1 d . C4B C 0.3394(5) 0.6877(5) 0.4043(2) 0.0164(10) Uani 1 1 d . H4BA H 0.2586 0.6695 0.4429 0.025 Uiso 1 1 calc GR H4BB H 0.2537 0.6097 0.3685 0.025 Uiso 1 1 calc GR H4BC H 0.4000 0.8190 0.3925 0.025 Uiso 1 1 calc GR C5B C 0.6714(5) 0.8871(5) 0.5063(2) 0.0179(10) Uani 1 1 d . H5BA H 0.7533 0.8949 0.5445 0.027 Uiso 1 1 calc GR H5BB H 0.5398 0.8695 0.5200 0.027 Uiso 1 1 calc GR H5BC H 0.7378 1.0025 0.4823 0.027 Uiso 1 1 calc GR C6B C 0.7737(5) 0.3879(5) 0.40597(19) 0.0132(10) Uani 1 1 d . H6B H 0.8878 0.4138 0.4324 0.016 Uiso 1 1 calc R C7B C 0.7198(5) 0.2336(5) 0.35937(19) 0.0128(9) Uani 1 1 d . C8B C 0.5573(5) 0.1715(5) 0.31584(19) 0.0155(9) Uani 1 1 d . H8B H 0.4699 0.2265 0.3167 0.019 Uiso 1 1 calc R C9B C 0.5237(5) 0.0279(5) 0.27089(19) 0.0147(9) Uani 1 1 d . H9B H 0.4145 -0.0125 0.2409 0.018 Uiso 1 1 calc R C10B C 0.6455(5) -0.0542(5) 0.2696(2) 0.0177(10) Uani 1 1 d . H10B H 0.6218 -0.1516 0.2391 0.021 Uiso 1 1 calc R C11B C 0.8039(5) 0.0057(5) 0.3132(2) 0.0125(9) Uani 1 1 d . C12B C 0.8443(5) 0.1477(4) 0.35795(19) 0.0133(9) Uani 1 1 d . H12B H 0.9548 0.1867 0.3873 0.016 Uiso 1 1 calc R 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 Br1A 0.0178(2) 0.0280(2) 0.0184(3) 0.0007(2) 0.0050(2) 0.0129(2) O1A 0.0219(16) 0.0185(15) 0.0205(19) 0.0063(13) 0.0032(13) 0.0133(13) N1A 0.0142(18) 0.0132(17) 0.0105(18) 0.0033(14) 0.0035(15) 0.0075(14) N2A 0.0136(18) 0.0100(16) 0.0139(19) 0.0011(15) 0.0016(16) 0.0071(14) C1A 0.013(2) 0.011(2) 0.013(2) -0.0036(19) 0.0015(19) 0.0023(18) C2A 0.011(2) 0.0122(19) 0.012(2) -0.0001(19) 0.0004(19) 0.0040(17) C3A 0.012(2) 0.011(2) 0.015(2) -0.0014(18) -0.0025(19) 0.0039(17) C4A 0.013(2) 0.015(2) 0.022(3) 0.0009(19) 0.0027(19) 0.0074(18) C5A 0.023(2) 0.015(2) 0.017(2) 0.0068(19) 0.005(2) 0.0072(19) C6A 0.010(2) 0.0085(19) 0.018(3) -0.0015(18) -0.0046(19) 0.0067(16) C7A 0.008(2) 0.0095(19) 0.014(2) -0.0022(18) -0.0042(17) 0.0014(17) C8A 0.011(2) 0.014(2) 0.021(3) 0.0005(19) 0.0034(19) 0.0063(18) C9A 0.012(2) 0.018(2) 0.016(2) 0.0030(19) -0.001(2) 0.0042(18) C10A 0.015(2) 0.015(2) 0.013(2) 0.0043(18) -0.0023(18) 0.0068(18) C11A 0.008(2) 0.012(2) 0.018(2) -0.0028(19) 0.0050(19) 0.0011(18) C12A 0.014(2) 0.011(2) 0.016(2) -0.0014(18) -0.0001(19) 0.0079(18) Br1B 0.0244(3) 0.0233(2) 0.0238(3) 0.0010(2) 0.0050(2) 0.0173(2) O1B 0.0169(15) 0.0144(14) 0.0196(17) -0.0019(13) -0.0040(14) 0.0072(12) N1B 0.0124(18) 0.0117(17) 0.014(2) -0.0011(15) 0.0004(16) 0.0061(14) N2B 0.0107(18) 0.0148(18) 0.017(2) 0.0009(15) 0.0007(15) 0.0068(15) C1B 0.013(2) 0.012(2) 0.016(3) 0.0090(18) 0.005(2) 0.0066(18) C2B 0.013(2) 0.009(2) 0.006(2) -0.0005(18) 0.0012(18) 0.0025(18) C3B 0.012(2) 0.015(2) 0.018(3) 0.009(2) 0.0057(19) 0.0052(19) C4B 0.016(2) 0.020(2) 0.014(2) 0.0038(19) 0.0016(19) 0.0099(19) C5B 0.015(2) 0.015(2) 0.024(3) -0.004(2) -0.005(2) 0.0070(18) C6B 0.009(2) 0.014(2) 0.012(2) 0.0060(19) -0.0033(18) 0.0014(18) C7B 0.012(2) 0.014(2) 0.013(2) 0.0034(18) 0.0044(18) 0.0067(18) C8B 0.015(2) 0.017(2) 0.018(2) 0.000(2) -0.001(2) 0.0102(17) C9B 0.013(2) 0.012(2) 0.015(2) 0.003(2) -0.001(2) 0.0028(18) C10B 0.018(2) 0.013(2) 0.020(3) 0.0003(19) 0.007(2) 0.0056(19) C11B 0.014(2) 0.015(2) 0.012(2) 0.005(2) 0.007(2) 0.0091(17) C12B 0.012(2) 0.014(2) 0.013(2) 0.0003(19) 0.0003(18) 0.0048(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C1A N1A C5A 123.5(3) C3A N1A C1A 108.5(3) C3A N1A C5A 128.0(3) C3A N2A C2A 104.9(3) O1A C1A N1A 126.5(4) O1A C1A C2A 131.5(4) N1A C1A C2A 102.0(3) N2A C2A C1A 110.0(3) C6A C2A N2A 128.7(4) C6A C2A C1A 121.3(4) N1A C3A C4A 120.7(3) N2A C3A N1A 114.5(3) N2A C3A C4A 124.8(3) C3A C4A H4AA 109.5 C3A C4A H4AB 109.5 C3A C4A H4AC 109.5 H4AA C4A H4AB 109.5 H4AA C4A H4AC 109.5 H4AB C4A H4AC 109.5 N1A C5A H5AA 109.5 N1A C5A H5AB 109.5 N1A C5A H5AC 109.5 H5AA C5A H5AB 109.5 H5AA C5A H5AC 109.5 H5AB C5A H5AC 109.5 C2A C6A H6A 115.3 C2A C6A C7A 129.4(4) C7A C6A H6A 115.3 C8A C7A C6A 124.6(3) C8A C7A C12A 118.5(3) C12A C7A C6A 117.0(3) C7A C8A H8A 119.3 C7A C8A C9A 121.3(4) C9A C8A H8A 119.3 C8A C9A H9A 119.8 C10A C9A C8A 120.3(4) C10A C9A H9A 119.8 C9A C10A H10A 120.7 C9A C10A C11A 118.5(4) C11A C10A H10A 120.7 C10A C11A Br1A 118.8(3) C12A C11A Br1A 119.0(3) C12A C11A C10A 122.1(3) C7A C12A H12A 120.4 C11A C12A C7A 119.2(4) C11A C12A H12A 120.4 C1B N1B C3B 108.2(3) C1B N1B C5B 123.5(3) C3B N1B C5B 128.3(3) C3B N2B C2B 105.1(3) O1B C1B N1B 125.7(4) O1B C1B C2B 131.1(4) N1B C1B C2B 103.2(3) N2B C2B C1B 109.8(3) C6B C2B N2B 129.6(4) C6B C2B C1B 120.6(4) N1B C3B C4B 120.9(4) N2B C3B N1B 113.7(4) N2B C3B C4B 125.4(4) C3B C4B H4BA 109.5 C3B C4B H4BB 109.5 C3B C4B H4BC 109.5 H4BA C4B H4BB 109.5 H4BA C4B H4BC 109.5 H4BB C4B H4BC 109.5 N1B C5B H5BA 109.5 N1B C5B H5BB 109.5 N1B C5B H5BC 109.5 H5BA C5B H5BB 109.5 H5BA C5B H5BC 109.5 H5BB C5B H5BC 109.5 C2B C6B H6B 114.6 C2B C6B C7B 130.8(4) C7B C6B H6B 114.6 C8B C7B C6B 124.2(4) C8B C7B C12B 119.0(4) C12B C7B C6B 116.7(4) C7B C8B H8B 120.1 C7B C8B C9B 119.8(4) C9B C8B H8B 120.1 C8B C9B H9B 119.6 C10B C9B C8B 120.8(4) C10B C9B H9B 119.6 C9B C10B H10B 120.4 C9B C10B C11B 119.1(4) C11B C10B H10B 120.4 C10B C11B Br1B 119.9(3) C10B C11B C12B 122.2(4) C12B C11B Br1B 117.9(3) C7B C12B H12B 120.5 C11B C12B C7B 118.9(4) C11B C12B H12B 120.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1A C11A 1.906(4) O1A C1A 1.214(4) N1A C1A 1.393(5) N1A C3A 1.381(4) N1A C5A 1.457(4) N2A C2A 1.400(4) N2A C3A 1.306(5) C1A C2A 1.490(5) C2A C6A 1.353(5) C3A C4A 1.489(5) C4A H4AA 0.9800 C4A H4AB 0.9800 C4A H4AC 0.9800 C5A H5AA 0.9800 C5A H5AB 0.9800 C5A H5AC 0.9800 C6A H6A 0.9500 C6A C7A 1.448(5) C7A C8A 1.384(5) C7A C12A 1.408(5) C8A H8A 0.9500 C8A C9A 1.388(5) C9A H9A 0.9500 C9A C10A 1.376(5) C10A H10A 0.9500 C10A C11A 1.387(5) C11A C12A 1.376(5) C12A H12A 0.9500 Br1B C11B 1.908(4) O1B C1B 1.216(4) N1B C1B 1.386(5) N1B C3B 1.396(5) N1B C5B 1.453(5) N2B C2B 1.408(5) N2B C3B 1.313(5) C1B C2B 1.475(5) C2B C6B 1.348(5) C3B C4B 1.480(5) C4B H4BA 0.9800 C4B H4BB 0.9800 C4B H4BC 0.9800 C5B H5BA 0.9800 C5B H5BB 0.9800 C5B H5BC 0.9800 C6B H6B 0.9500 C6B C7B 1.461(5) C7B C8B 1.398(5) C7B C12B 1.402(5) C8B H8B 0.9500 C8B C9B 1.401(5) C9B H9B 0.9500 C9B C10B 1.359(5) C10B H10B 0.9500 C10B C11B 1.379(5) C11B C12B 1.380(5) C12B H12B 0.9500 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 Br1A C11A C12A C7A -179.2(3) O1A C1A C2A N2A -179.9(4) O1A C1A C2A C6A 0.0(6) N1A C1A C2A N2A 0.0(4) N1A C1A C2A C6A 179.9(3) N2A C2A C6A C7A 0.7(6) C1A N1A C3A N2A -0.4(4) C1A N1A C3A C4A -179.4(3) C1A C2A C6A C7A -179.2(3) C2A N2A C3A N1A 0.4(4) C2A N2A C3A C4A 179.3(3) C2A C6A C7A C8A 0.2(6) C2A C6A C7A C12A 179.9(4) C3A N1A C1A O1A -179.9(4) C3A N1A C1A C2A 0.2(4) C3A N2A C2A C1A -0.2(4) C3A N2A C2A C6A 179.9(4) C5A N1A C1A O1A 0.3(6) C5A N1A C1A C2A -179.6(3) C5A N1A C3A N2A 179.4(3) C5A N1A C3A C4A 0.4(5) C6A C7A C8A C9A 178.9(3) C6A C7A C12A C11A -179.6(3) C7A C8A C9A C10A 0.0(6) C8A C7A C12A C11A 0.0(5) C8A C9A C10A C11A 1.4(5) C9A C10A C11A Br1A 178.5(3) C9A C10A C11A C12A -2.1(6) C10A C11A C12A C7A 1.4(6) C12A C7A C8A C9A -0.7(5) Br1B C11B C12B C7B -179.3(3) O1B C1B C2B N2B -179.7(4) O1B C1B C2B C6B -0.2(6) N1B C1B C2B N2B 1.2(4) N1B C1B C2B C6B -179.3(3) N2B C2B C6B C7B 0.8(7) C1B N1B C3B N2B 0.0(4) C1B N1B C3B C4B -179.7(3) C1B C2B C6B C7B -178.5(3) C2B N2B C3B N1B 0.8(4) C2B N2B C3B C4B -179.5(3) C2B C6B C7B C8B -0.1(6) C2B C6B C7B C12B 178.1(4) C3B N1B C1B O1B -179.9(3) C3B N1B C1B C2B -0.7(4) C3B N2B C2B C1B -1.3(4) C3B N2B C2B C6B 179.4(4) C5B N1B C1B O1B 0.5(6) C5B N1B C1B C2B 179.7(3) C5B N1B C3B N2B 179.6(3) C5B N1B C3B C4B -0.2(6) C6B C7B C8B C9B 176.9(3) C6B C7B C12B C11B -177.7(3) C7B C8B C9B C10B 1.0(6) C8B C7B C12B C11B 0.6(5) C8B C9B C10B C11B -0.1(6) C9B C10B C11B Br1B 179.0(3) C9B C10B C11B C12B -0.5(6) C10B C11B C12B C7B 0.3(6) C12B C7B C8B C9B -1.2(5) loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.4952(6) 2 0.5048(6)