#------------------------------------------------------------------------------ #$Date: 2025-01-18 03:19:11 +0200 (Sat, 18 Jan 2025) $ #$Revision: 297374 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573716.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_1573716 _journal_paper_doi 10.1039/D4OB01942C _chemical_formula_sum 'C10 H11 Br O Se' _chemical_formula_weight 306.05 _chemical_name_common 6-bromo-3,6-dimethyl-5,6-dihydrobenzo[b]selenophen-7(4H)-one _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 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2024-10-30 deposited with the CCDC. 2025-01-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.80(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.767(3) _cell_length_b 10.906(4) _cell_length_c 12.122(4) _cell_measurement_reflns_used 1907 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 24.83 _cell_measurement_theta_min 3.10 _cell_volume 1026.7(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6465 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.680 _diffrn_reflns_theta_min 3.095 _exptl_absorpt_coefficient_mu 7.506 _exptl_absorpt_correction_T_max 0.399 _exptl_absorpt_correction_T_min 0.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.980 _exptl_crystal_description prism _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.150 _refine_diff_density_max 0.615 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.022 _refine_ls_R_factor_all 0.0602 _refine_ls_R_factor_gt 0.0376 _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^)+(0.0417P)^2^+1.4504P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.0884 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1496 _reflns_number_total 1949 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ob01942c3.cif _cod_data_source_block compound2 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1573716 _shelx_shelxl_version_number 2014/7 _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 0.315 _shelx_estimated_absorpt_t_max 0.399 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL Jp02_a.res in P2(1)/n CELL 0.71073 7.7669 10.9057 12.1220 90.000 90.803 90.000 ZERR 2.00 0.0028 0.0035 0.0036 0.000 0.020 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H O SE BR UNIT 40 44 4 4 4 MERG 2 OMIT 0.00 180.00 shel 8 0.82 MPLA SE1 C2 C3 C7A C3A FMAP 2 PLAN 20 SIZE 0.150 0.150 0.200 ACTA BOND $H LIST 4 L.S. 20 TEMP 23.00 WGHT 0.041700 1.450400 FVAR 0.43048 BR1 5 0.085209 0.480957 0.734137 11.00000 0.03021 0.04249 = 0.04920 0.00641 0.00622 -0.00044 SE1 4 0.657008 0.285443 0.812188 11.00000 0.03606 0.03493 = 0.05725 0.00172 0.00229 0.01171 O1 3 0.396013 0.308657 0.611862 11.00000 0.04628 0.04305 = 0.05407 -0.02345 -0.00339 -0.00142 C2 1 0.745527 0.396313 0.913295 11.00000 0.02340 0.05551 = 0.04504 0.00537 0.00055 0.00365 AFIX 43 H2 2 0.829695 0.376033 0.965483 11.00000 -1.20000 AFIX 0 C3 1 0.676267 0.509943 0.904245 11.00000 0.02909 0.04214 = 0.02968 -0.00006 0.00339 -0.00948 C4 1 0.444614 0.631392 0.795795 11.00000 0.03611 0.02212 = 0.03975 0.00214 0.00216 -0.00408 AFIX 23 H4A 2 0.516608 0.703241 0.806314 11.00000 -1.20000 H4B 2 0.350397 0.636445 0.847284 11.00000 -1.20000 AFIX 0 C5 1 0.372618 0.630810 0.678737 11.00000 0.03269 0.02973 = 0.03955 0.00591 0.00028 -0.00308 AFIX 23 H5A 2 0.287063 0.695286 0.672136 11.00000 -1.20000 H5B 2 0.465059 0.650431 0.628732 11.00000 -1.20000 AFIX 0 C6 1 0.291190 0.511389 0.642154 11.00000 0.02202 0.03726 = 0.03424 0.00273 0.00434 -0.00439 C7 1 0.404048 0.400191 0.667840 11.00000 0.02460 0.03835 = 0.03300 -0.00237 0.00735 -0.00454 C7A 1 0.521170 0.414470 0.760887 11.00000 0.02877 0.02681 = 0.03304 0.00243 0.00485 -0.00143 C3A 1 0.547908 0.519112 0.819721 11.00000 0.02683 0.02973 = 0.02717 0.00445 0.00498 -0.00322 C8 1 0.729058 0.615812 0.975268 11.00000 0.04258 0.06235 = 0.03502 0.00132 -0.00537 -0.01387 AFIX 33 H8A 2 0.663432 0.686968 0.954529 11.00000 -1.50000 H8B 2 0.708253 0.596402 1.051168 11.00000 -1.50000 H8C 2 0.849406 0.632087 0.965739 11.00000 -1.50000 AFIX 0 C9 1 0.233256 0.513274 0.518311 11.00000 0.02875 0.04457 = 0.04024 0.00867 -0.01108 -0.00283 AFIX 33 H9A 2 0.182554 0.435745 0.499103 11.00000 -1.50000 H9B 2 0.150186 0.577355 0.506805 11.00000 -1.50000 H9C 2 0.331406 0.527881 0.472877 11.00000 -1.50000 AFIX 0 HKLF 4 REM Jp02_a.res in P2(1)/n REM R1 = 0.0376 for 1496 Fo > 4sig(Fo) and 0.0602 for all 1949 data REM 118 parameters refined using 0 restraints END WGHT 0.0417 1.4504 REM Highest difference peak 0.615, deepest hole -0.542, 1-sigma level 0.105 Q1 1 0.6892 0.3189 0.8656 11.00000 0.05 0.62 Q2 1 0.7251 0.2390 0.7828 11.00000 0.05 0.60 Q3 1 0.6354 0.6264 1.0030 11.00000 0.05 0.49 Q4 1 0.2781 0.4856 0.4834 11.00000 0.05 0.48 Q5 1 0.1865 0.4762 0.5334 11.00000 0.05 0.43 Q6 1 0.8110 0.5744 1.0357 11.00000 0.05 0.42 Q7 1 0.2137 0.5616 0.5193 11.00000 0.05 0.42 Q8 1 0.2642 0.5367 0.5505 11.00000 0.05 0.41 Q9 1 0.6469 0.3238 0.7624 11.00000 0.05 0.40 Q10 1 0.5670 0.3186 0.8471 11.00000 0.05 0.38 Q11 1 0.2600 0.4813 0.5547 11.00000 0.05 0.38 Q12 1 0.1918 0.5000 0.6816 11.00000 0.05 0.38 Q13 1 0.1631 0.5401 0.6981 11.00000 0.05 0.36 Q14 1 0.2349 0.4445 0.8181 11.00000 0.05 0.35 Q15 1 0.7962 0.6803 0.9377 11.00000 0.05 0.34 Q16 1 -0.0584 0.4781 0.6589 11.00000 0.05 0.33 Q17 1 0.6453 0.5249 0.9272 11.00000 0.05 0.31 Q18 1 0.0299 0.5386 0.7949 11.00000 0.05 0.30 Q19 1 0.5983 0.6953 1.0198 11.00000 0.05 0.30 Q20 1 0.5642 0.3614 0.7558 11.00000 0.05 0.29 ; _shelx_res_checksum 98337 _shelx_hkl_file ; 1 0 0 1.30 0.70 -1 0 0 -0.40 0.70 -1 0 0 0.70 0.50 1 0 0 0.60 0.60 2 0 0 69.29 4.10 2 0 0 85.29 4.10 -2 0 0 74.89 5.10 -2 0 0 81.99 4.30 -3 0 0 -6.00 4.10 3 0 0 -2.40 2.90 -3 0 0 -3.50 2.90 4 0 0 1480.05 36.60 -4 0 0 1512.85 38.00 -4 0 0 1499.05 37.10 -5 0 0 -15.70 7.10 5 0 0 -8.20 4.70 -5 0 0 2.80 5.00 -6 0 0 107.59 11.50 -7 0 0 -13.00 11.00 -8 0 0 29.40 13.20 -9 0 0 -5.10 14.10 0 -1 0 -2.30 0.20 0 1 0 -1.80 0.30 1 -1 0 12.90 1.50 1 -1 0 22.10 2.20 -1 1 0 10.10 1.70 -1 1 0 21.40 2.10 2 -1 0 1924.01 46.80 2 -1 0 2036.10 47.10 -2 1 0 2035.90 47.20 -2 1 0 2009.80 47.10 3 -1 0 100.29 7.10 -3 1 0 111.69 7.00 -3 1 0 101.29 6.70 4 -1 0 475.25 15.20 -4 -1 0 437.46 15.30 -4 1 0 467.35 16.30 -4 1 0 467.85 15.20 5 -1 0 993.30 26.80 -5 -1 0 946.01 27.20 -5 -1 0 933.21 25.80 -5 1 0 947.91 28.40 -6 -1 0 33.10 6.40 -6 -1 0 19.00 9.00 6 -1 0 24.30 7.40 -6 1 0 34.80 10.20 -7 -1 0 267.57 19.00 7 -1 0 277.77 16.00 -7 1 0 303.57 20.90 -8 -1 0 185.28 15.60 -8 1 0 181.98 16.50 -9 -1 0 9.90 13.70 -9 1 0 29.40 15.30 0 -2 0 1614.04 37.50 0 2 0 1602.54 37.40 1 -2 0 234.08 7.90 1 -2 0 247.78 7.20 -1 -2 0 237.88 6.20 -1 2 0 234.18 7.70 1 2 0 236.78 6.30 -1 2 0 233.28 8.10 -1 2 0 240.88 7.40 2 -2 0 524.75 15.80 2 -2 0 552.74 15.20 -2 2 0 604.14 16.00 -2 2 0 561.14 15.80 3 -2 0 92.09 6.80 -3 2 0 99.09 6.60 -3 2 0 95.19 7.30 4 -2 0 222.08 11.70 -4 2 0 222.58 12.70 5 -2 0 122.29 9.40 -5 2 0 103.39 10.90 6 -2 0 1742.53 46.10 -6 2 0 1749.43 47.70 7 -2 0 108.19 11.70 -7 2 0 119.49 14.40 -8 2 0 72.09 15.30 -9 -2 0 33.00 13.50 -9 2 0 52.69 16.30 0 -3 0 -1.50 1.80 0 3 0 1.90 2.00 1 -3 0 4304.87 100.99 1 -3 0 4357.16 100.19 -1 -3 0 4434.06 99.59 -1 3 0 4355.26 100.99 -1 3 0 4473.75 100.09 1 3 0 4419.86 99.59 -2 -3 0 206.18 6.20 2 -3 0 202.38 8.00 2 -3 0 203.28 9.30 -2 3 0 191.58 8.80 3 -3 0 641.54 19.70 -3 3 0 643.24 19.50 4 -3 0 866.91 26.20 -4 3 0 915.21 26.50 5 -3 0 684.43 23.40 -5 3 0 705.53 24.50 6 -3 0 53.99 9.80 -6 3 0 29.30 11.50 7 -3 0 32.50 10.40 -7 3 0 64.99 13.60 8 -3 0 155.48 14.80 -8 3 0 156.48 18.10 -9 3 0 14.10 16.50 0 -4 0 3238.48 75.69 0 4 0 3262.37 75.29 1 -4 0 1083.99 27.10 -1 -4 0 1028.80 25.30 1 -4 0 1030.30 25.80 -1 4 0 1043.10 25.70 -1 4 0 1051.29 28.00 1 4 0 1047.70 25.30 2 -4 0 5.20 3.30 2 -4 0 -3.70 4.40 -2 -4 0 3.80 1.80 -2 4 0 0.60 4.40 -3 -4 0 414.46 11.50 3 -4 0 385.96 15.50 -3 4 0 405.16 15.20 4 -4 0 630.84 22.20 -4 -4 0 689.23 18.00 -4 4 0 663.23 22.40 5 -4 0 200.28 15.20 -5 4 0 221.88 16.40 6 -4 0 38.00 10.30 -6 4 0 3.70 11.50 7 -4 0 26.00 11.10 -7 4 0 29.70 14.10 8 -4 0 66.09 13.40 -8 4 0 82.59 16.90 -9 4 0 25.40 17.90 0 5 0 1.30 3.30 -1 -5 0 62.29 4.30 1 -5 0 53.29 6.00 1 -5 0 57.99 4.50 -1 5 0 60.39 6.60 -1 5 0 57.09 4.70 1 5 0 65.09 4.70 2 -5 0 702.73 21.30 -2 -5 0 677.03 17.80 2 -5 0 710.43 23.50 -2 5 0 702.23 22.90 2 5 0 682.53 17.80 -2 5 0 712.93 20.00 -3 -5 0 1127.69 27.60 3 -5 0 1126.39 31.70 -3 5 0 1117.59 30.70 -4 -5 0 14.90 3.10 4 -5 0 -2.90 7.20 -4 5 0 -1.20 8.10 5 -5 0 577.74 23.10 -5 -5 0 550.74 17.10 -5 5 0 559.94 23.40 6 -5 0 35.80 11.10 -6 5 0 37.30 12.70 7 -5 0 458.75 24.70 -7 5 0 471.05 27.40 8 -5 0 34.70 13.40 -8 5 0 24.50 16.50 -9 5 0 122.69 20.10 0 6 0 700.93 19.70 1 -6 0 165.78 7.70 1 -6 0 130.19 9.60 -1 -6 0 146.49 6.90 1 6 0 146.79 6.90 -1 6 0 129.49 9.80 -2 -6 0 49.00 4.00 2 -6 0 34.10 6.90 -2 6 0 45.10 6.10 -2 6 0 45.60 8.40 2 6 0 46.80 4.40 3 -6 0 555.14 20.90 -3 -6 0 569.44 15.90 -3 6 0 626.44 23.30 -3 6 0 603.74 19.90 -4 -6 0 37.90 4.10 4 -6 0 29.30 9.10 -4 6 0 23.70 9.20 5 -6 0 650.73 26.10 -5 6 0 683.13 26.10 6 -6 0 256.57 17.50 -6 6 0 242.48 17.70 7 -6 0 198.98 17.30 -7 6 0 136.39 17.70 8 -6 0 132.09 16.70 -8 6 0 74.39 18.20 0 7 0 -2.90 4.30 1 -7 0 767.92 21.50 -1 -7 0 781.22 21.80 1 -7 0 742.43 23.30 -1 7 0 830.32 24.60 1 7 0 793.62 21.30 -2 -7 0 131.89 6.70 2 -7 0 111.09 9.90 -2 7 0 113.79 8.10 -2 7 0 127.29 11.70 2 7 0 120.79 7.20 -3 -7 0 388.86 12.40 3 -7 0 389.66 18.30 -3 7 0 436.56 20.40 -3 7 0 413.66 16.80 4 -7 0 68.29 10.80 -4 -7 0 65.19 5.50 -4 7 0 68.29 10.60 -4 7 0 58.99 12.30 5 -7 0 65.19 12.40 -5 7 0 64.79 12.60 6 -7 0 20.90 12.30 -6 7 0 22.10 13.50 7 -7 0 38.80 14.20 -7 7 0 51.49 16.40 8 -7 0 114.89 17.40 -8 7 0 129.09 20.30 0 8 0 355.56 13.70 -1 -8 0 730.83 21.60 1 -8 0 732.03 21.10 1 -8 0 731.43 23.30 1 8 0 720.63 20.80 -1 8 0 754.42 24.10 -2 -8 0 37.00 4.90 2 -8 0 24.70 8.30 2 8 0 33.80 5.10 -2 8 0 18.40 8.60 3 -8 0 412.16 19.60 -3 -8 0 420.26 13.50 -3 8 0 433.76 21.60 -3 8 0 410.76 17.50 4 -8 0 -8.40 10.00 -4 8 0 13.60 11.00 -4 8 0 9.60 9.60 5 -8 0 77.69 13.50 -5 8 0 74.59 14.60 -5 8 0 94.69 13.50 6 -8 0 201.88 17.70 -6 8 0 188.98 17.60 -6 8 0 150.58 19.20 7 -8 0 25.20 15.10 -7 8 0 10.00 16.40 -7 8 0 31.90 16.60 0 9 0 0.30 5.60 1 -9 0 64.49 9.50 1 -9 0 61.39 7.20 -1 9 0 81.99 9.70 1 9 0 78.89 7.10 2 -9 0 137.59 12.30 -2 9 0 126.99 13.00 2 9 0 124.49 8.30 3 -9 0 302.57 19.60 -3 9 0 335.67 20.50 -3 9 0 299.57 16.00 4 -9 0 424.56 24.10 -4 9 0 416.76 20.60 -4 9 0 405.36 24.20 5 -9 0 69.69 14.60 -5 9 0 61.79 15.40 -5 9 0 63.59 13.40 6 -9 0 34.30 14.90 -6 9 0 30.60 16.20 -6 9 0 41.00 14.90 7 -9 0 137.39 18.40 -7 9 0 104.79 18.40 -7 9 0 88.09 18.90 0 10 0 670.83 22.00 1 -10 0 17.40 9.10 -1 10 0 40.60 9.00 1 10 0 35.50 6.40 2 -10 0 16.20 10.30 2 10 0 26.60 5.90 -2 10 0 15.50 9.70 3 -10 0 85.19 13.30 -3 10 0 69.09 13.40 4 -10 0 44.10 13.70 -4 10 0 35.60 11.20 -4 10 0 50.39 14.40 5 -10 0 265.07 19.90 -5 10 0 217.18 16.80 -5 10 0 151.88 18.60 6 -10 0 11.30 15.40 -6 10 0 11.00 14.80 -6 10 0 5.10 15.90 0 11 0 2.20 6.70 1 -11 0 53.49 11.50 1 11 0 48.10 7.50 -1 11 0 51.09 9.90 2 -11 0 313.97 21.60 -2 11 0 252.67 18.50 2 11 0 276.77 12.90 3 -11 0 57.79 14.60 -3 11 0 55.69 13.50 4 -11 0 5.30 13.90 -4 11 0 6.10 12.70 5 -11 0 48.10 16.30 -5 11 0 16.40 15.40 0 12 0 81.39 9.80 1 -12 0 135.29 14.90 -1 12 0 89.39 11.90 1 12 0 113.29 10.20 2 -12 0 24.30 13.50 -2 12 0 27.80 11.00 2 12 0 32.40 9.90 3 -12 0 371.86 26.60 -3 12 0 271.97 22.00 4 -12 0 64.79 17.10 -4 12 0 45.30 15.00 0 13 0 -2.40 8.20 1 -13 0 -16.10 12.80 -1 13 0 1.30 9.50 2 -13 0 32.30 15.10 -2 13 0 15.20 11.40 -3 13 0 10.60 12.70 -8 0 1 4.20 12.80 -7 0 1 599.14 24.80 -6 0 1 -6.50 9.10 5 0 -1 1914.91 48.30 -5 0 1 2034.40 49.10 -5 0 1 1947.91 49.80 -4 0 1 -1.40 5.40 -4 0 1 4.50 4.20 4 0 -1 -3.70 4.50 -3 0 1 1080.49 27.80 -3 0 1 1108.99 27.90 3 0 -1 1105.69 27.70 -2 0 1 -1.70 2.60 -2 0 1 -4.50 2.40 2 0 -1 -5.30 2.70 2 0 -1 -1.70 1.90 -1 0 1 145.19 4.70 1 0 -1 159.28 5.10 0 0 -1 -11.40 0.30 0 0 1 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14.40 -2 -5 12 11.00 12.40 2 -5 -12 5.50 10.50 -2 5 12 -1.30 12.70 -2 5 12 3.20 13.20 -1 -5 12 35.00 13.10 1 -5 -12 39.30 10.10 1 5 -12 40.80 10.20 -1 5 12 76.29 13.10 -1 5 12 53.29 14.70 0 -5 12 69.69 13.50 0 -5 -12 61.89 10.50 0 5 -12 65.89 10.30 0 5 12 72.89 18.90 0 5 12 83.89 13.90 1 -5 12 -15.10 11.90 -1 -5 -12 13.00 9.00 -1 5 -12 -8.00 9.50 1 5 12 13.10 12.10 -2 -5 -12 8.60 9.00 2 -5 12 -8.10 12.50 -2 5 -12 -0.50 10.10 -3 -5 -12 4.70 9.50 3 -5 12 -5.20 13.20 -3 5 -12 0.40 11.70 -4 -5 -12 53.79 11.60 4 -5 12 11.30 15.00 -4 5 -12 21.00 13.00 -4 -6 12 55.89 16.00 4 -6 -12 87.09 15.60 -4 6 12 46.00 18.40 -4 6 12 67.09 17.80 3 -6 -12 19.50 12.10 -3 -6 12 25.60 14.20 -3 6 12 13.20 15.60 -3 6 12 29.30 14.70 -2 -6 12 20.30 13.40 2 -6 -12 21.20 11.60 -2 6 12 -7.50 13.90 -2 6 12 28.90 14.30 1 -6 -12 16.50 10.00 -1 -6 12 18.40 13.10 -1 6 12 6.50 13.60 0 -6 12 -9.40 12.90 0 -6 -12 -7.70 9.40 0 6 12 -7.60 12.00 -1 -6 -12 -0.80 9.20 1 -6 12 -5.40 13.00 -1 6 -12 -17.70 9.50 1 6 12 9.70 12.50 -2 -6 -12 19.60 10.10 2 -6 12 11.40 14.10 -2 6 -12 22.70 10.80 3 -6 12 20.90 15.50 -3 -6 -12 37.90 10.60 -3 6 -12 39.10 12.60 -4 -6 -12 21.90 11.10 -4 6 -12 17.30 13.40 -3 -7 12 20.20 15.10 3 -7 -12 -5.00 12.70 -3 7 12 0.30 16.20 2 -7 -12 9.30 12.00 -2 -7 12 10.20 14.70 -2 7 12 1.60 15.20 -1 -7 12 1.10 13.90 1 -7 -12 16.20 11.20 -1 7 12 9.90 15.00 0 -7 -12 9.70 10.30 0 -7 12 11.50 14.10 0 7 12 22.40 13.70 -1 -7 -12 83.19 11.70 1 -7 12 79.99 16.00 1 7 12 80.69 15.40 2 -7 12 -18.30 14.80 -2 -7 -12 -6.10 9.70 -3 -7 -12 27.80 11.10 3 -7 12 22.50 16.20 -3 7 -12 15.00 12.70 2 -8 -12 -9.50 12.20 -2 8 12 11.80 16.60 1 -8 -12 109.39 14.10 -1 -8 12 100.09 16.90 -1 8 12 71.39 17.40 0 -8 12 5.60 15.10 0 -8 -12 2.80 11.00 0 8 12 20.10 14.90 -1 -8 -12 32.50 11.40 1 -8 12 32.10 16.40 1 8 12 46.10 14.80 -5 0 13 77.89 17.70 -4 0 13 5.40 15.00 4 0 -13 0.70 10.80 -4 0 13 14.00 11.60 -3 0 13 90.59 12.90 3 0 -13 86.79 12.20 -3 0 13 98.89 15.30 2 0 -13 -4.60 9.50 -2 0 13 8.40 10.90 -2 0 13 1.30 12.50 -1 0 13 -4.90 11.10 1 0 -13 -1.90 9.50 0 0 13 -2.90 10.90 0 0 -13 -3.50 9.50 1 0 13 77.79 12.40 -1 0 -13 52.89 11.00 -2 0 -13 11.80 10.60 2 0 13 -8.00 10.70 3 0 13 -0.30 10.50 -3 0 -13 5.80 11.00 -4 0 -13 -22.00 11.30 -5 -1 13 21.80 17.50 -5 1 13 27.60 14.10 -5 1 13 13.90 17.10 4 -1 -13 18.00 11.60 -4 -1 13 41.10 15.60 -4 1 13 27.70 15.50 -4 1 13 37.90 13.60 3 -1 -13 -5.00 10.20 -3 -1 13 13.00 13.70 -3 1 13 -10.00 11.50 -3 1 13 8.30 14.10 3 1 -13 -1.70 9.60 -2 -1 13 57.99 13.10 2 -1 -13 66.19 11.30 -2 1 13 69.29 12.80 2 1 -13 50.59 10.30 -2 1 13 64.49 13.70 -1 -1 13 -5.90 11.80 1 -1 -13 7.80 9.60 -1 1 13 1.20 11.60 1 1 -13 -8.80 9.10 0 -1 -13 128.49 12.50 0 -1 13 152.78 14.20 0 1 13 140.19 13.70 0 1 -13 118.99 12.50 -1 -1 -13 57.79 10.80 1 -1 13 52.09 12.10 1 1 13 40.80 11.40 -1 1 -13 49.50 11.10 2 -1 13 -13.20 10.80 -2 -1 -13 3.60 10.10 2 1 13 0.20 10.50 -2 1 -13 -14.60 10.30 -3 -1 -13 0.70 10.80 3 -1 13 -11.70 10.80 3 1 13 -24.70 15.40 -3 1 -13 -1.10 11.00 4 -1 13 -6.00 11.70 -4 -1 -13 3.90 11.30 -4 1 -13 -7.00 12.40 5 -2 -13 13.40 12.80 -5 2 13 51.79 15.70 4 -2 -13 -5.80 11.40 -4 -2 13 -16.60 14.50 -4 2 13 -3.90 13.20 -4 2 13 -8.90 15.10 -3 -2 13 14.30 13.30 3 -2 -13 5.50 11.00 -3 2 13 4.20 13.00 3 2 -13 4.50 9.80 -3 2 13 7.30 14.00 2 -2 -13 -0.90 9.90 -2 -2 13 4.00 12.90 -2 2 13 10.40 12.00 2 2 -13 -12.30 9.10 -2 2 13 7.50 12.90 1 -2 -13 139.79 13.00 -1 -2 13 144.29 14.90 1 2 -13 139.89 12.60 -1 2 13 139.89 15.10 -1 2 13 129.59 14.40 0 -2 13 -3.50 11.80 0 -2 -13 -4.80 9.50 0 2 -13 -5.50 9.20 0 2 13 6.10 11.10 1 -2 13 91.09 13.40 -1 -2 -13 63.89 11.40 1 2 13 71.59 12.10 -1 2 -13 56.79 11.50 2 -2 13 25.20 12.00 -2 -2 -13 38.60 10.80 2 2 13 18.50 10.40 -2 2 -13 19.20 11.40 -3 -2 -13 36.00 11.20 3 -2 13 54.19 13.50 -3 2 -13 46.20 12.40 -4 -2 -13 -6.10 10.80 4 -2 13 -20.60 12.00 -4 2 -13 -19.70 12.00 4 -3 -13 -13.40 12.10 -4 -3 13 -14.40 14.80 -4 3 13 8.70 14.70 -4 3 13 -23.00 15.60 3 -3 -13 46.20 12.70 -3 -3 13 56.39 14.90 -3 3 13 57.69 15.10 -3 3 13 63.49 15.70 -2 -3 13 95.69 14.90 2 -3 -13 67.09 12.10 -2 3 13 61.09 14.20 2 3 -13 63.29 10.90 -2 3 13 91.49 15.00 1 -3 -13 54.69 11.30 -1 -3 13 65.69 13.80 -1 3 13 65.69 13.50 1 3 -13 54.79 10.60 -1 3 13 59.89 13.40 0 -3 -13 42.80 10.50 0 -3 13 29.60 12.70 0 3 13 27.50 11.90 0 3 -13 27.60 10.20 0 3 13 50.09 13.10 -1 -3 -13 74.29 11.30 1 -3 13 56.99 13.40 -1 3 -13 51.79 11.50 1 3 13 54.09 11.60 -2 -3 -13 0.10 9.80 2 -3 13 -2.00 12.30 -2 3 -13 11.70 11.20 -3 -3 -13 15.60 10.70 3 -3 13 -9.10 12.80 -3 3 -13 -8.30 11.60 4 -3 13 1.40 13.30 -4 -3 -13 3.70 11.10 -4 3 -13 -5.10 13.00 -4 -4 13 10.50 15.40 4 -4 -13 2.00 13.10 -4 4 13 -8.20 15.70 -4 4 13 11.60 16.80 -3 -4 13 11.90 14.70 3 -4 -13 11.50 12.50 -3 4 13 16.60 15.40 -3 4 13 14.70 14.70 -2 -4 13 -0.30 13.70 2 -4 -13 10.10 11.30 -2 4 13 -7.90 13.70 -2 4 13 9.00 14.20 -1 -4 13 20.90 13.20 1 -4 -13 12.20 10.50 1 4 -13 -4.20 9.40 -1 4 13 9.60 12.90 -1 4 13 10.70 12.40 0 -4 13 30.80 13.40 0 -4 -13 1.00 10.00 0 4 13 7.20 12.50 0 4 13 -8.70 11.20 0 4 -13 6.00 9.80 1 -4 13 4.50 13.00 -1 -4 -13 18.30 10.40 -1 4 -13 10.60 10.80 2 -4 13 4.90 13.20 -2 -4 -13 -0.30 9.60 -2 4 -13 -3.30 11.20 -3 -4 -13 21.90 11.00 3 -4 13 1.40 14.00 -3 4 -13 -5.80 12.20 -4 -4 -13 26.30 11.70 -4 4 -13 2.90 13.90 3 -5 -13 -4.80 12.20 -3 -5 13 7.70 14.90 -3 5 13 -5.10 15.50 -3 5 13 -22.10 15.00 -2 -5 13 48.40 15.20 2 -5 -13 38.50 12.40 -2 5 13 38.60 15.50 -2 5 13 63.49 15.50 -1 -5 13 -15.60 13.90 1 -5 -13 -5.50 10.50 -1 5 13 -5.90 13.60 0 -5 -13 142.99 13.70 0 -5 13 168.88 17.20 0 5 -13 125.59 12.70 0 5 13 154.08 17.50 1 -5 13 -10.30 13.70 -1 -5 -13 4.10 10.10 -1 5 -13 -4.90 10.30 2 -5 13 19.40 14.60 -2 -5 -13 24.20 10.70 -2 5 -13 14.70 11.60 3 -5 13 15.00 15.10 -3 -5 -13 35.00 11.30 -3 5 -13 16.30 13.10 2 -6 -13 113.49 15.00 -2 -6 13 148.09 17.90 -2 6 13 110.59 18.50 1 -6 -13 38.30 12.10 -1 -6 13 24.00 15.60 -1 6 13 28.00 15.50 0 -6 13 -9.10 14.90 0 -6 -13 7.00 10.60 0 6 13 -3.50 14.20 1 -6 13 19.20 15.60 -1 -6 -13 8.90 10.50 1 6 13 43.50 14.90 2 -6 13 48.40 16.50 -2 -6 -13 50.69 11.50 -2 6 -13 35.60 12.60 1 -7 -13 -8.30 11.90 -1 7 13 -20.40 15.50 0 -7 13 10.60 15.90 0 -7 -13 1.80 11.20 0 7 13 12.30 15.30 -1 -7 -13 3.80 10.80 3 0 -14 -1.10 11.10 -3 0 14 6.60 12.30 -3 0 14 -18.10 14.80 2 0 -14 53.89 12.00 -2 0 14 67.49 15.50 1 0 -14 -5.70 10.60 -1 0 14 1.50 12.80 0 0 14 99.19 14.60 0 0 -14 73.89 12.60 -1 0 -14 1.10 11.00 1 0 14 -12.50 11.90 -2 0 -14 59.49 12.90 2 0 14 83.69 13.80 -3 0 -14 4.70 12.30 -3 -1 14 58.59 15.90 3 -1 -14 42.90 12.50 3 1 -14 24.50 11.50 -3 1 14 46.30 16.00 -3 1 14 49.60 13.60 2 -1 -14 -9.80 10.50 -2 -1 14 9.80 14.00 -2 1 14 4.20 12.60 -2 1 14 -4.30 14.00 2 1 -14 -10.30 10.20 1 -1 -14 64.89 12.50 -1 -1 14 91.59 15.20 -1 1 14 72.29 15.00 1 1 -14 51.89 11.60 0 -1 -14 19.00 11.40 0 -1 14 17.80 13.50 0 1 14 20.70 12.70 0 1 -14 11.80 11.30 1 -1 14 8.30 12.80 -1 -1 -14 24.60 11.50 -1 1 -14 15.80 11.40 1 1 14 10.90 11.70 -2 -1 -14 13.30 11.80 2 -1 14 27.60 13.10 -2 1 -14 12.40 12.20 2 1 14 19.60 12.10 -3 -1 -14 34.10 13.30 3 -1 14 16.80 13.00 -3 1 -14 24.40 13.00 3 -2 -14 -2.50 12.20 -3 -2 14 -10.90 15.20 -3 2 14 2.80 15.40 -3 2 14 7.60 13.70 2 -2 -14 7.60 11.50 -2 -2 14 -6.40 14.00 -2 2 14 -5.50 14.30 -2 2 14 -1.10 13.10 2 2 -14 -0.60 10.40 1 -2 -14 3.10 11.00 -1 -2 14 12.80 14.00 1 2 -14 0.50 10.20 -1 2 14 -27.10 12.60 0 -2 14 -10.40 13.00 0 -2 -14 12.80 11.20 0 2 -14 -3.40 10.70 0 2 14 2.50 12.20 1 -2 14 2.80 13.20 -1 -2 -14 9.10 11.30 1 2 14 5.60 12.00 -1 2 -14 0.80 11.40 2 -2 14 7.90 13.20 -2 -2 -14 -0.10 11.30 -2 2 -14 6.20 12.60 3 -2 14 2.30 13.30 -3 -2 -14 3.80 11.80 -3 2 -14 4.00 12.60 3 -3 -14 84.29 14.80 -3 -3 14 132.29 18.00 -3 3 14 82.59 17.40 -3 3 14 111.59 18.00 -2 -3 14 1.70 15.00 2 -3 -14 -12.80 11.30 -2 3 14 -13.00 13.50 -2 3 14 -13.70 14.20 1 -3 -14 6.70 11.30 -1 -3 14 8.20 14.20 1 3 -14 6.70 10.90 -1 3 14 2.80 13.20 -1 3 14 -7.70 13.20 0 -3 14 -17.80 13.60 0 -3 -14 -6.10 10.80 0 3 -14 -12.00 10.60 0 3 14 12.20 12.20 1 -3 14 89.89 15.30 -1 -3 -14 53.79 12.60 -1 3 -14 57.49 12.50 -2 -3 -14 19.20 11.60 2 -3 14 27.20 14.80 -2 3 -14 22.40 13.00 -3 -3 -14 -8.50 11.40 -3 3 -14 -2.00 12.80 -2 -4 14 46.20 16.10 2 -4 -14 45.20 13.50 -2 4 14 41.20 16.10 -2 4 14 76.69 16.50 -1 -4 14 50.39 16.10 1 -4 -14 36.00 12.10 -1 4 14 40.60 14.70 -1 4 14 53.09 15.60 0 -4 14 -4.60 14.30 0 -4 -14 8.00 11.30 0 4 -14 4.00 10.70 0 4 14 14.30 14.60 -1 -4 -14 -4.30 11.00 1 -4 14 -8.50 14.40 -1 4 -14 -5.20 11.20 2 -4 14 90.39 17.00 -2 -4 -14 80.49 12.90 -2 4 -14 72.39 14.30 1 -5 -14 0.70 11.70 -1 -5 14 -0.80 15.40 -1 5 14 3.40 14.90 0 -5 14 11.90 15.80 0 -5 -14 35.60 12.50 0 5 14 40.30 15.40 -1 -5 -14 1.20 11.40 -1 5 -14 -3.20 11.60 2 0 -15 -6.60 12.00 -1 0 15 -16.10 15.10 1 0 -15 -0.90 12.10 0 0 15 -13.50 14.00 0 0 -15 -6.30 11.70 -1 0 -15 22.20 13.20 1 0 15 37.00 14.80 1 -1 -15 -9.60 11.90 -1 -1 15 -13.20 14.90 -1 1 15 -16.30 14.40 1 1 -15 -0.80 11.50 0 -1 -15 23.30 12.80 0 -1 15 1.90 14.70 0 1 15 23.20 14.70 0 1 -15 20.80 12.80 1 -1 15 -7.50 14.40 -1 -1 -15 -10.30 12.30 -1 1 -15 14.30 12.50 1 1 15 3.60 13.10 1 -2 -15 62.69 13.90 1 2 -15 61.89 13.20 0 -2 15 4.70 15.30 0 -2 -15 -12.80 11.90 0 2 15 -13.60 14.00 0 2 -15 4.30 12.50 -1 -2 -15 28.20 13.00 -1 2 -15 4.70 12.80 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 74395 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 Br1 Br 0.08521(6) 0.48096(5) 0.73414(4) 0.04058(18) Uani 1 1 d . . . . . Se1 Se 0.65701(7) 0.28544(5) 0.81219(4) 0.04273(18) Uani 1 1 d . . . . . O1 O 0.3960(5) 0.3087(3) 0.6119(3) 0.0478(10) Uani 1 1 d . . . . . C2 C 0.7455(6) 0.3963(5) 0.9133(4) 0.0413(13) Uani 1 1 d . . . . . H2 H 0.8297 0.3760 0.9655 0.050 Uiso 1 1 calc R U . . . C3 C 0.6763(6) 0.5099(5) 0.9042(4) 0.0336(11) Uani 1 1 d . . . . . C4 C 0.4446(6) 0.6314(4) 0.7958(4) 0.0326(11) Uani 1 1 d . . . . . H4A H 0.5166 0.7032 0.8063 0.039 Uiso 1 1 calc R U . . . H4B H 0.3504 0.6364 0.8473 0.039 Uiso 1 1 calc R U . . . C5 C 0.3726(6) 0.6308(4) 0.6787(4) 0.0340(11) Uani 1 1 d . . . . . H5A H 0.2871 0.6953 0.6721 0.041 Uiso 1 1 calc R U . . . H5B H 0.4651 0.6504 0.6287 0.041 Uiso 1 1 calc R U . . . C6 C 0.2912(6) 0.5114(4) 0.6422(4) 0.0311(11) Uani 1 1 d . . . . . C7 C 0.4040(6) 0.4002(5) 0.6678(4) 0.0319(11) Uani 1 1 d . . . . . C7A C 0.5212(6) 0.4145(4) 0.7609(4) 0.0295(10) Uani 1 1 d . . . . . C3A C 0.5479(6) 0.5191(4) 0.8197(3) 0.0279(10) Uani 1 1 d . . . . . C8 C 0.7291(7) 0.6158(5) 0.9753(4) 0.0467(14) Uani 1 1 d . . . . . H8A H 0.6634 0.6870 0.9545 0.070 Uiso 1 1 calc R U . . . H8B H 0.7083 0.5964 1.0512 0.070 Uiso 1 1 calc R U . . . H8C H 0.8494 0.6321 0.9657 0.070 Uiso 1 1 calc R U . . . C9 C 0.2333(6) 0.5133(5) 0.5183(4) 0.0380(12) Uani 1 1 d . . . . . H9A H 0.1826 0.4357 0.4991 0.057 Uiso 1 1 calc R U . . . H9B H 0.1502 0.5774 0.5068 0.057 Uiso 1 1 calc R U . . . H9C H 0.3314 0.5279 0.4729 0.057 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0302(3) 0.0425(3) 0.0492(3) 0.0064(2) 0.0062(2) -0.0004(2) Se1 0.0361(3) 0.0349(3) 0.0573(3) 0.0017(2) 0.0023(2) 0.0117(3) O1 0.046(2) 0.043(2) 0.054(2) -0.0234(18) -0.0034(18) -0.0014(19) C2 0.023(3) 0.056(4) 0.045(3) 0.005(3) 0.001(2) 0.004(3) C3 0.029(3) 0.042(3) 0.030(2) 0.000(2) 0.0034(19) -0.009(2) C4 0.036(3) 0.022(2) 0.040(3) 0.002(2) 0.002(2) -0.004(2) C5 0.033(3) 0.030(3) 0.040(3) 0.006(2) 0.000(2) -0.003(2) C6 0.022(2) 0.037(3) 0.034(2) 0.003(2) 0.0043(19) -0.004(2) C7 0.025(3) 0.038(3) 0.033(2) -0.002(2) 0.0073(19) -0.005(2) C7A 0.029(3) 0.027(2) 0.033(2) 0.002(2) 0.0049(19) -0.001(2) C3A 0.027(3) 0.030(3) 0.027(2) 0.0045(19) 0.0050(18) -0.003(2) C8 0.043(3) 0.062(4) 0.035(3) 0.001(3) -0.005(2) -0.014(3) C9 0.029(3) 0.045(3) 0.040(3) 0.009(2) -0.011(2) -0.003(2) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' 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 C2 Se1 C7A 86.0(2) . . ? C3 C2 Se1 113.7(4) . . ? C3 C2 H2 123.2 . . ? Se1 C2 H2 123.2 . . ? C2 C3 C3A 113.3(4) . . ? C2 C3 C8 123.7(5) . . ? C3A C3 C8 123.0(5) . . ? C3A C4 C5 111.6(4) . . ? C3A C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3A C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C6 C5 C4 115.2(4) . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 C7 112.8(4) . . ? C5 C6 C9 112.6(4) . . ? C7 C6 C9 111.3(4) . . ? C5 C6 Br1 108.4(3) . . ? C7 C6 Br1 102.5(3) . . ? C9 C6 Br1 108.5(3) . . ? O1 C7 C7A 123.6(5) . . ? O1 C7 C6 121.1(4) . . ? C7A C7 C6 115.2(4) . . ? C3A C7A C7 126.1(4) . . ? C3A C7A Se1 112.2(3) . . ? C7 C7A Se1 121.8(3) . . ? C7A C3A C3 114.8(4) . . ? C7A C3A C4 120.6(4) . . ? C3 C3A C4 124.6(4) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C6 1.991(4) . ? Se1 C2 1.847(5) . ? Se1 C7A 1.860(5) . ? O1 C7 1.208(6) . ? C2 C3 1.355(7) . ? C2 H2 0.9300 . ? C3 C3A 1.423(6) . ? C3 C8 1.494(7) . ? C4 C3A 1.490(6) . ? C4 C5 1.518(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.512(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.526(7) . ? C6 C9 1.561(6) . ? C7 C7A 1.447(6) . ? C7A C3A 1.360(6) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ?