#------------------------------------------------------------------------------ #$Date: 2024-11-21 01:07:39 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296016 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573213.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_1573213 loop_ _publ_author_name 'Chen, Ci' 'Zhang, Qiaoya' 'Huang, Zhiwei' 'Ouyang, Wensen' 'Gao, Yang' 'Luo, Jiye' 'Liu, Yuan' 'Huo, Yanping' 'Chen, Qian' 'Li, Xianwei' _publ_section_title ; Ru(ii)-catalyzed regioselective oxidative Heck reaction with internal olefins that tolerated strongly coordinating heterocycles ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07036D _journal_year 2024 _chemical_absolute_configuration rm _chemical_formula_moiety 'C10 H8 Br N O2 S' _chemical_formula_sum 'C10 H8 Br N O2 S' _chemical_formula_weight 286.14 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-05-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-06-05 deposited with the CCDC. 2024-11-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 3.99710(10) _cell_length_b 7.0195(2) _cell_length_c 40.9871(10) _cell_measurement_reflns_used 9171 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.14 _cell_measurement_theta_min 2.94 _cell_volume 1150.00(5) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 297.97 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.936 _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 0.0440 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 0.945 _diffrn_reflns_Laue_measured_fraction_max 0.936 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_number 7436 _diffrn_reflns_point_group_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.277 _diffrn_reflns_theta_min 2.944 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.734 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.5298 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0991 before and 0.0745 after correction. The Ratio of minimum to maximum transmission is 0.7107. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 568 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.270 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Flack x determined using 791 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.044(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2426 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.0805 _reflns_Friedel_coverage 0.636 _reflns_Friedel_fraction_full 0.958 _reflns_Friedel_fraction_max 0.950 _reflns_number_gt 2194 _reflns_number_total 2426 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07036d2.cif _cod_data_source_block mo_20240527_lixw_0ma_a _cod_database_code 1573213 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C8(H8) 2.b Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C10(H10A,H10B,H10C) ; _shelx_res_file ; TITL mo_20240527_Lixw_0ma_a.res in P2(1)2(1)2(1) mo_20240527_lixw_0ma_a.res created by SHELXL-2018/3 at 15:45:26 on 27-May-2024 REM Old TITL mo_20240527_Lixw_0ma in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.138, Rweak 0.077, Alpha 0.004, Orientation as input REM Flack x = 0.105 ( 0.009 ) from Parsons' quotients REM Formula found by SHELXT: C9 N2 O2 S Br CELL 0.71073 3.9971 7.0195 40.9871 90 90 90 ZERR 4 0.0001 0.0002 0.001 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S Br UNIT 40 32 4 8 4 4 L.S. 10 PLAN 20 TEMP 24.82 BOND $H LIST 6 fmap 2 acta OMIT 1 1 5 REM REM REM WGHT 0.028600 FVAR 1.24716 BR1 6 0.292753 1.113442 0.472716 11.00000 0.06793 0.06551 = 0.06543 -0.02870 0.00498 0.00142 S002 5 0.573443 0.718789 0.453520 11.00000 0.05783 0.05261 = 0.04441 0.00092 -0.00448 0.00292 O2 4 0.161861 0.371511 0.306559 11.00000 0.10159 0.06178 = 0.04837 -0.01269 -0.01024 -0.00416 O1 4 0.352764 0.645221 0.286225 11.00000 0.13854 0.09086 = 0.04381 0.00812 -0.00199 -0.02967 N1 3 0.854706 0.323485 0.399789 11.00000 0.07300 0.03967 = 0.08579 0.00712 0.00742 0.01372 C2 1 0.365096 0.945586 0.408983 11.00000 0.04686 0.03035 = 0.05140 -0.00041 -0.00163 0.00307 AFIX 43 H2 2 0.277337 1.052680 0.398726 11.00000 -1.20000 AFIX 0 C4 1 0.590664 0.645332 0.413462 11.00000 0.04134 0.03296 = 0.04607 0.00152 -0.00201 0.00355 C1 1 0.406777 0.931584 0.441575 11.00000 0.04373 0.04377 = 0.05328 -0.00716 0.00181 -0.00131 C3 1 0.469242 0.779769 0.392032 11.00000 0.03704 0.03014 = 0.04810 -0.00044 -0.00157 -0.00090 C6 1 0.449010 0.757800 0.355975 11.00000 0.04238 0.04100 = 0.04506 0.00551 0.00187 0.00505 C5 1 0.734019 0.464333 0.405708 11.00000 0.05087 0.03327 = 0.05528 0.00721 0.00304 0.00732 C8 1 0.340631 0.592164 0.344018 11.00000 0.05879 0.04102 = 0.03833 0.00062 0.00256 0.00123 AFIX 43 H8 2 0.292230 0.496820 0.359049 11.00000 -1.20000 AFIX 0 C9 1 0.290033 0.545482 0.309229 11.00000 0.06756 0.05714 = 0.03938 0.00007 0.00011 0.00421 C7 1 0.543345 0.929870 0.336536 11.00000 0.08128 0.05100 = 0.06057 0.01556 -0.00018 -0.01146 AFIX 137 H7A 2 0.479385 1.042671 0.348219 11.00000 -1.50000 H7B 2 0.430395 0.926795 0.315873 11.00000 -1.50000 H7C 2 0.780821 0.930614 0.333038 11.00000 -1.50000 AFIX 0 C10 1 0.084680 0.306629 0.274065 11.00000 0.11486 0.09214 = 0.05947 -0.02449 -0.01544 -0.00517 AFIX 137 H10A 2 0.284150 0.308171 0.261021 11.00000 -1.50000 H10B 2 -0.079539 0.389283 0.264487 11.00000 -1.50000 H10C 2 -0.001988 0.179209 0.275038 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_20240527_Lixw_0ma_a.res in P2(1)2(1)2(1) REM wR2 = 0.0805, GooF = S = 1.031, Restrained GooF = 1.031 for all data REM R1 = 0.0317 for 2194 Fo > 4sig(Fo) and 0.0360 for all 2426 data REM 138 parameters refined using 0 restraints END WGHT 0.0281 0.0000 REM Highest difference peak 0.270, deepest hole -0.370, 1-sigma level 0.050 Q1 1 0.4363 1.0389 0.4781 11.00000 0.05 0.27 Q2 1 -0.1006 1.0987 0.4758 11.00000 0.05 0.23 Q3 1 0.0385 1.2232 0.4721 11.00000 0.05 0.21 Q4 1 0.2810 1.0598 0.3336 11.00000 0.05 0.20 Q5 1 0.7071 1.0976 0.4743 11.00000 0.05 0.20 Q6 1 0.2252 1.0728 0.4413 11.00000 0.05 0.19 Q7 1 0.3071 0.5895 0.4511 11.00000 0.05 0.18 Q8 1 0.2981 0.2142 0.2740 11.00000 0.05 0.18 Q9 1 1.0074 0.7206 0.4604 11.00000 0.05 0.18 Q10 1 0.2066 1.2273 0.4447 11.00000 0.05 0.18 Q11 1 -0.0067 1.0351 0.4750 11.00000 0.05 0.17 Q12 1 0.7067 1.0189 0.3470 11.00000 0.05 0.16 Q13 1 0.6975 0.8705 0.3058 11.00000 0.05 0.16 Q14 1 0.3557 0.9420 0.4304 11.00000 0.05 0.16 Q15 1 0.3033 1.0346 0.5072 11.00000 0.05 0.15 Q16 1 0.2382 0.5148 0.2747 11.00000 0.05 0.15 Q17 1 0.2366 0.6479 0.4001 11.00000 0.05 0.14 Q18 1 0.4848 1.2374 0.4478 11.00000 0.05 0.14 Q19 1 0.6323 0.8888 0.3187 11.00000 0.05 0.14 Q20 1 0.4530 0.7064 0.4825 11.00000 0.05 0.14 ; _shelx_res_checksum 49364 _shelx_hkl_file ; 0 -1 0 0.20 1.00 0 1 0 1.20 1.60 0 2 0 543.05 48.00 0 -2 0 577.64 48.10 0 3 0 -2.40 4.00 0 -3 0 0.20 3.80 0 4 0 4295.17 363.06 0 -4 0 4466.95 362.86 0 5 0 6.20 7.90 0 -5 0 3.20 8.10 0 -6 0 1021.10 93.69 0 6 0 1097.39 95.09 0 -7 0 8.10 13.20 0 -8 0 57.69 19.10 0 -9 0 1.80 16.70 1 2 0 5955.10 482.35 1 -2 0 5877.21 482.15 -1 2 0 5780.12 482.15 -1 -2 0 5849.02 482.15 1 3 0 1416.46 121.49 1 -3 0 1445.46 121.19 -1 3 0 1462.55 121.29 1 -4 0 1523.35 125.99 1 4 0 1564.04 126.49 -1 -4 0 1390.56 125.59 -1 4 0 1460.95 125.99 1 5 0 536.05 50.69 1 -5 0 523.45 50.19 -1 -5 0 551.14 50.09 -1 5 0 521.15 50.39 1 6 0 189.58 24.60 1 -6 0 175.58 24.10 -1 6 0 110.09 20.20 -1 -6 0 170.48 23.90 1 -7 0 13.90 13.70 -1 7 0 4.90 11.40 -1 -7 0 9.60 13.60 1 -8 0 10.70 13.50 -1 -8 0 1.00 14.60 2 -1 0 974.50 77.39 2 1 0 967.60 77.39 -2 1 0 928.41 77.39 -2 -1 0 857.31 77.29 2 2 0 3059.49 255.97 2 -2 0 3181.78 256.07 -2 -2 0 3061.19 255.77 2 3 0 99.89 13.90 2 -3 0 100.99 13.80 -2 -3 0 105.99 13.70 -2 3 0 105.89 13.80 2 4 0 2815.62 243.18 2 -4 0 2748.32 242.68 -2 -4 0 2972.50 242.48 -2 4 0 3115.49 243.28 2 5 0 362.96 37.10 -2 -5 0 346.37 35.90 2 -6 0 -2.30 11.60 -2 -6 0 7.00 10.30 -2 6 0 1.60 9.60 2 -7 0 43.90 15.80 -2 -7 0 49.00 16.40 -2 7 0 57.59 17.90 2 -8 0 30.40 16.30 -2 -8 0 34.20 17.50 3 2 0 2235.88 176.68 3 -2 0 2190.48 176.68 -3 2 0 2141.59 176.68 -3 -2 0 1977.80 176.48 3 3 0 5.80 6.90 3 -3 0 -2.30 3.50 -3 -3 0 3.80 6.30 -3 3 0 4.20 5.80 3 4 0 -1.60 7.30 3 -4 0 6.50 8.80 -3 -4 0 -1.80 7.50 -3 4 0 -1.50 7.70 3 -5 0 566.24 54.09 -3 5 0 547.95 53.29 -3 -5 0 611.94 53.69 3 -6 0 101.89 19.60 -3 6 0 110.99 20.30 -3 -6 0 117.49 19.50 3 -7 0 67.99 19.60 -3 -7 0 74.79 18.20 -3 7 0 76.99 18.10 -4 3 0 91.09 11.60 -4 3 0 80.89 12.10 4 4 0 8.10 7.20 4 -4 0 2.50 7.70 -4 4 0 5.40 6.60 -4 -4 0 2.70 7.80 4 -5 0 3.20 10.70 -4 5 0 26.10 10.40 -4 -5 0 21.50 10.20 0 -9 1 1.40 16.00 0 -8 1 5.20 15.00 0 -7 1 271.47 44.60 0 6 -1 220.78 28.60 0 -6 1 236.38 29.00 0 -5 1 2848.62 236.58 0 5 -1 2796.12 236.98 0 -4 1 0.60 6.60 0 4 -1 1.80 5.50 0 2 -1 4.60 3.40 0 -2 1 4.70 3.20 0 -1 1 263.87 22.60 0 -1 -1 276.17 23.70 0 -2 -1 5.90 3.70 0 2 1 5.70 3.20 0 -4 -1 0.90 5.50 0 4 1 -1.00 6.00 0 -5 -1 2862.31 237.18 0 5 1 2798.52 237.58 0 6 1 220.68 29.10 0 -6 -1 233.48 28.30 0 -7 -1 175.28 28.40 0 -8 -1 -0.40 14.60 0 -9 -1 -2.00 16.80 1 -8 1 14.20 15.20 -1 -8 1 12.20 15.80 1 -7 1 66.69 19.70 -1 7 -1 81.69 19.20 -1 -7 1 117.79 20.70 1 -6 1 1382.16 108.89 1 6 -1 1352.56 109.29 -1 -6 1 1113.69 107.09 -1 6 -1 1089.59 107.49 1 5 -1 855.81 74.49 1 -5 1 884.81 74.29 -1 -5 1 809.12 73.59 -1 5 -1 760.72 73.69 1 -4 1 898.51 73.09 1 4 -1 896.21 73.29 -1 4 -1 781.22 72.39 -1 -4 1 755.12 72.09 1 -3 1 54.59 8.80 1 3 -1 43.50 8.80 -1 3 -1 74.39 10.40 1 1 -1 2183.78 182.58 -1 1 -1 2156.18 182.58 -1 -1 1 2310.77 182.48 1 1 1 2417.76 198.68 -1 -1 -1 2408.26 198.68 1 -3 -1 77.69 11.20 1 3 1 80.19 11.40 -1 3 1 66.99 11.00 1 -4 -1 804.82 76.09 1 4 1 813.62 76.59 -1 -4 -1 921.91 76.49 -1 4 1 973.10 77.09 1 5 1 814.72 73.79 1 -5 -1 810.62 73.49 -1 5 1 805.02 73.49 -1 -5 -1 857.01 73.49 1 -6 -1 1191.68 109.49 1 6 1 1155.58 109.99 -1 -6 -1 1366.76 110.09 -1 6 1 1297.07 110.59 1 -7 -1 98.69 20.10 -1 7 1 97.69 20.40 -1 -7 -1 99.79 20.20 1 -8 -1 -0.60 13.10 -1 -8 -1 5.20 14.20 2 -8 1 3.10 15.70 -2 -8 1 23.30 16.80 2 -7 1 212.98 30.80 -2 7 -1 205.98 32.00 -2 -7 1 198.88 29.70 2 -6 1 50.79 15.70 -2 -6 1 52.79 14.20 -2 6 -1 39.30 12.90 2 5 -1 7.80 10.00 -2 -5 1 31.10 10.70 -2 5 -1 38.70 12.90 2 4 -1 898.71 83.29 2 -4 1 913.91 83.19 -2 4 -1 1028.90 83.59 -2 -4 1 984.80 82.89 2 -3 1 964.10 85.19 2 3 -1 907.21 84.89 -2 3 -1 1068.19 85.09 -2 -3 1 1041.40 84.79 2 2 -1 1310.17 114.99 2 -2 1 1324.27 115.19 -2 -2 1 1285.07 114.69 -2 2 -1 1602.04 115.39 2 -1 1 7888.71 651.23 -2 -1 1 7668.33 650.93 -2 1 -1 8269.97 651.23 2 1 1 8061.79 647.14 -2 1 1 8028.10 647.04 -2 -1 -1 7588.54 647.14 2 2 1 1437.36 113.89 2 -2 -1 1213.68 113.39 -2 2 1 1544.65 113.89 -2 -2 -1 1257.67 113.39 2 3 1 971.00 81.79 2 -3 -1 937.31 81.39 -2 -3 -1 912.51 81.19 -2 3 1 992.40 81.69 2 4 1 930.91 82.39 2 -4 -1 909.21 81.89 -2 -4 -1 948.01 81.79 -2 4 1 982.80 82.29 2 -5 -1 40.30 14.40 2 5 1 32.40 11.00 -2 -5 -1 6.30 8.40 2 -6 -1 77.49 16.80 -2 -6 -1 36.80 13.50 -2 6 1 55.29 14.80 2 -7 -1 201.38 30.40 -2 -7 -1 204.68 28.90 -2 7 1 211.48 30.40 2 -8 -1 29.50 16.60 -2 -8 -1 11.10 16.70 3 -7 1 32.50 16.80 -3 7 -1 14.70 12.70 -3 -7 1 30.60 14.20 3 -6 1 16.30 12.10 -3 6 -1 14.80 11.10 -3 -6 1 3.60 10.80 3 -5 1 149.29 21.70 -3 5 -1 139.89 20.30 -3 -5 1 156.88 21.20 3 4 -1 54.09 11.80 3 -4 1 43.90 11.80 -3 4 -1 59.39 12.60 -3 -4 1 55.99 11.40 3 3 -1 291.77 26.60 3 -3 1 288.17 27.20 -3 -3 1 240.28 26.00 -3 3 -1 266.47 26.30 3 2 -1 2768.82 200.98 3 -2 1 2479.85 199.88 -3 2 -1 2324.47 199.78 -3 -2 1 2118.29 199.38 3 2 1 2405.46 191.78 3 -2 -1 2227.08 191.38 -3 -2 -1 2286.17 191.68 -3 2 1 2358.66 191.58 3 3 1 310.97 28.30 -3 3 1 294.87 27.60 -3 -3 -1 267.17 27.60 3 -4 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212.58 37.60 0 -4 44 46.90 19.60 0 4 -44 33.70 19.80 0 3 -44 80.59 22.40 0 2 -44 8.30 13.60 0 1 -44 140.99 24.80 0 0 -44 169.48 30.70 0 -1 -44 113.19 22.40 0 -2 -44 10.60 12.30 0 -3 -44 114.59 23.90 0 -4 -44 31.70 15.90 0 -5 -44 253.77 37.40 1 4 -44 199.58 32.20 -1 4 -44 172.38 33.70 1 3 -44 9.50 16.00 -1 3 -44 26.40 18.20 1 2 -44 13.30 17.30 -1 2 -44 11.40 15.60 1 1 -44 134.69 23.10 -1 1 -44 89.49 20.20 1 0 -44 222.28 33.60 -1 0 -44 236.98 34.40 1 -1 -44 137.19 25.10 -1 -1 -44 142.39 26.20 1 -2 -44 16.80 13.20 -1 2 44 16.20 12.20 -1 -2 -44 19.80 14.90 1 -3 -44 26.70 18.90 -1 -3 -44 32.50 18.20 1 -4 -44 179.68 30.70 -1 -4 -44 220.78 34.30 2 3 -44 46.30 19.00 -2 3 -44 59.79 21.90 2 2 -44 79.69 19.80 -2 2 -44 99.49 25.30 2 1 -44 115.19 21.80 -2 1 -44 105.29 26.00 2 0 -44 13.60 13.00 -2 0 -44 27.80 18.40 2 -1 -44 81.49 18.90 -2 -1 -44 110.79 23.30 2 -2 -44 105.69 22.20 -2 -2 -44 100.99 25.20 2 -3 -44 64.39 21.00 -2 -3 -44 43.70 19.70 -2 3 44 60.69 16.80 0 4 -45 -8.10 17.30 0 3 -45 80.29 22.40 0 2 -45 258.97 35.40 0 1 -45 78.79 21.30 0 0 -45 15.10 15.40 0 -1 -45 93.59 21.60 0 -2 -45 250.67 34.50 0 -3 -45 79.69 19.40 0 -4 -45 -5.70 15.00 1 4 -45 77.79 23.20 -1 4 -45 81.99 26.10 1 3 -45 72.39 21.20 -1 3 -45 101.99 24.50 1 2 -45 0.00 14.00 -1 2 -45 10.10 16.80 1 1 -45 199.78 30.40 -1 1 -45 151.78 28.10 1 0 -45 46.70 18.60 -1 0 -45 42.70 19.10 1 -1 -45 158.38 28.10 -1 -1 -45 179.38 28.30 1 -2 -45 20.50 15.80 -1 2 45 -1.80 11.70 -1 -2 -45 9.20 15.60 1 -3 -45 118.59 24.00 -1 -3 -45 101.69 26.60 1 -4 -45 69.29 20.40 -1 -4 -45 74.49 23.30 2 3 -45 14.20 15.10 -2 3 -45 34.60 18.50 2 2 -45 145.39 27.20 -2 2 -45 159.78 27.40 2 1 -45 14.00 15.00 -2 1 -45 31.00 20.20 2 0 -45 30.20 15.20 -2 0 -45 10.90 16.60 2 -1 -45 34.80 17.20 -2 -1 -45 27.40 17.90 2 -2 -45 194.78 27.90 -2 -2 -45 138.09 28.70 2 -3 -45 25.20 16.80 -2 -3 -45 11.80 21.10 -2 3 45 7.40 13.70 0 4 -46 5.60 17.70 0 3 -46 23.00 18.20 0 2 -46 -4.70 13.00 0 1 -46 112.59 21.60 0 0 -46 136.99 26.80 0 -1 -46 156.38 27.10 0 -2 -46 -5.00 15.00 0 -3 -46 13.60 12.10 0 -4 -46 12.40 15.20 1 4 -46 128.39 29.70 -1 4 -46 146.59 30.10 1 3 -46 41.50 18.40 -1 3 -46 50.69 20.30 1 2 -46 40.00 15.90 -1 2 -46 33.80 15.50 1 1 -46 -1.70 15.70 -1 1 -46 4.30 16.00 1 0 -46 46.40 18.90 -1 0 -46 44.10 19.40 1 -1 -46 3.40 12.90 -1 -1 -46 -2.70 14.20 1 -2 -46 45.00 17.10 -1 -2 -46 54.09 19.60 1 -3 -46 80.79 20.90 -1 -3 -46 55.19 20.40 1 -4 -46 152.78 26.50 -1 -4 -46 196.18 32.10 2 2 -46 46.10 18.10 -2 2 -46 66.69 25.20 2 1 -46 96.99 23.10 -2 1 -46 60.79 20.70 2 0 -46 0.70 12.60 -2 0 -46 11.30 16.90 2 -1 -46 59.99 17.40 -2 -1 -46 101.29 23.50 2 -2 -46 40.70 17.10 -2 -2 -46 76.09 25.30 0 4 -47 -7.00 17.80 0 3 -47 34.10 19.90 0 2 -47 421.06 49.30 0 1 -47 239.38 36.70 0 0 -47 26.10 17.70 0 -1 -47 171.78 27.90 0 -2 -47 404.06 47.20 0 -3 -47 30.90 17.40 0 -4 -47 2.10 14.50 1 3 -47 20.50 17.70 -1 3 -47 52.59 22.80 1 2 -47 84.29 24.40 -1 2 -47 43.70 22.60 1 1 -47 109.39 23.10 -1 1 -47 112.79 22.80 1 0 -47 135.59 27.30 -1 0 -47 180.08 30.50 1 -1 -47 105.19 24.50 -1 -1 -47 162.78 27.60 1 -2 -47 38.90 17.60 -1 -2 -47 91.79 24.00 1 -3 -47 53.39 18.10 -1 -3 -47 18.30 16.30 2 2 -47 12.10 17.60 -2 2 -47 31.00 17.70 2 1 -47 3.40 15.80 -2 1 -47 39.60 21.10 2 0 -47 1.40 13.30 -2 0 -47 -0.40 17.30 2 -1 -47 27.00 17.80 -2 -1 -47 18.40 20.10 2 -2 -47 32.60 16.40 -2 -2 -47 22.90 19.90 0 3 -48 3.30 15.20 0 2 -48 28.90 16.40 0 1 -48 20.00 17.10 0 0 -48 1.30 15.40 0 -1 -48 8.10 13.50 0 -2 -48 40.20 18.30 0 -3 -48 13.10 17.60 1 3 -48 25.10 18.90 -1 3 -48 75.19 24.10 1 2 -48 73.89 21.60 -1 2 -48 64.69 19.50 1 1 -48 64.79 24.60 -1 1 -48 75.29 23.50 -1 0 -48 171.78 30.80 1 -1 -48 93.19 26.30 -1 -1 -48 80.19 22.90 1 -2 -48 74.89 21.70 -1 -2 -48 69.09 21.50 1 -3 -48 49.00 18.40 -1 -3 -48 62.79 21.60 2 1 -48 31.90 16.00 -2 1 -48 77.39 27.20 2 0 -48 98.29 22.10 2 -1 -48 37.50 15.30 -2 -1 -48 33.90 21.20 0 3 -49 4.60 14.60 0 2 -49 125.69 24.90 0 1 -49 8.60 15.80 0 0 -49 25.70 18.80 0 -1 -49 17.20 15.50 0 -2 -49 199.08 32.60 0 -3 -49 4.80 14.40 1 2 -49 88.09 20.70 -1 2 -49 76.89 25.00 1 1 -49 61.09 20.50 -1 1 -49 141.89 29.10 1 0 -49 129.89 26.30 -1 0 -49 164.18 31.00 1 -1 -49 108.39 24.00 -1 -1 -49 106.19 25.10 1 -2 -49 78.99 19.80 -1 -2 -49 172.88 30.50 0 2 -50 33.90 19.80 0 1 -50 128.59 29.40 0 0 -50 252.57 37.50 0 -1 -50 112.39 26.50 0 -2 -50 18.80 17.20 1 2 -50 49.00 22.60 -1 2 -50 28.00 20.30 1 1 -50 42.60 18.90 -1 1 -50 52.19 19.80 1 0 -50 -5.60 15.30 -1 0 -50 -5.00 17.20 1 -1 -50 49.90 17.60 -1 -1 -50 55.89 21.50 1 -2 -50 31.00 19.30 -1 -2 -50 49.50 21.20 0 2 -51 31.00 17.70 0 1 -51 4.60 15.20 0 0 -51 20.50 16.80 0 -1 -51 1.70 16.60 0 -2 -51 81.19 24.90 1 1 -51 27.10 20.50 -1 1 -51 47.20 21.70 1 0 -51 34.70 18.10 -1 0 -51 53.09 21.10 1 -1 -51 29.80 17.70 -1 -1 -51 48.50 20.50 0 1 -52 9.90 18.90 0 0 -52 105.89 24.60 0 -1 -52 4.20 17.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 88587 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.29275(13) 1.11344(7) 0.47272(2) 0.06629(19) Uani 1 1 d . . . . . S002 S 0.5734(3) 0.71879(16) 0.45352(2) 0.0516(3) Uani 1 1 d . . . . . O2 O 0.1619(10) 0.3715(5) 0.30656(7) 0.0706(9) Uani 1 1 d . . . . . O1 O 0.3528(13) 0.6452(5) 0.28623(8) 0.0911(13) Uani 1 1 d . . . . . N1 N 0.8547(12) 0.3235(5) 0.39979(11) 0.0662(11) Uani 1 1 d . . . . . C2 C 0.3651(10) 0.9456(5) 0.40898(9) 0.0429(8) Uani 1 1 d . . . . . H2 H 0.277337 1.052680 0.398726 0.051 Uiso 1 1 calc R . . . . C4 C 0.5907(9) 0.6453(5) 0.41346(8) 0.0401(7) Uani 1 1 d . . . . . C1 C 0.4068(10) 0.9316(5) 0.44157(9) 0.0469(9) Uani 1 1 d . . . . . C3 C 0.4692(9) 0.7798(5) 0.39203(8) 0.0384(7) Uani 1 1 d . . . . . C6 C 0.4490(10) 0.7578(5) 0.35598(9) 0.0428(8) Uani 1 1 d . . . . . C5 C 0.7340(11) 0.4643(5) 0.40571(9) 0.0465(8) Uani 1 1 d . . . . . C8 C 0.3406(10) 0.5922(5) 0.34402(9) 0.0460(8) Uani 1 1 d . . . . . H8 H 0.292230 0.496820 0.359049 0.055 Uiso 1 1 calc R . . . . C9 C 0.2900(12) 0.5455(6) 0.30923(9) 0.0547(10) Uani 1 1 d . . . . . C7 C 0.5433(14) 0.9299(6) 0.33654(11) 0.0643(12) Uani 1 1 d . . . . . H7A H 0.479385 1.042671 0.348219 0.096 Uiso 1 1 calc GR . . . . H7B H 0.430395 0.926795 0.315873 0.096 Uiso 1 1 calc GR . . . . H7C H 0.780821 0.930614 0.333038 0.096 Uiso 1 1 calc GR . . . . C10 C 0.0847(19) 0.3066(9) 0.27406(12) 0.0888(19) Uani 1 1 d . . . . . H10A H 0.284150 0.308171 0.261021 0.133 Uiso 1 1 calc GR . . . . H10B H -0.079539 0.389283 0.264487 0.133 Uiso 1 1 calc GR . . . . H10C H -0.001988 0.179209 0.275038 0.133 Uiso 1 1 calc GR . . . . 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 0.0679(3) 0.0655(3) 0.0654(3) -0.0287(2) 0.0050(2) 0.0014(2) S002 0.0578(6) 0.0526(6) 0.0444(5) 0.0009(4) -0.0045(4) 0.0029(4) O2 0.102(2) 0.0618(19) 0.0484(16) -0.0127(14) -0.0102(15) -0.004(2) O1 0.139(4) 0.091(3) 0.0438(17) 0.0081(18) -0.0020(19) -0.030(3) N1 0.073(3) 0.0397(19) 0.086(3) 0.0071(18) 0.007(2) 0.0137(17) C2 0.047(2) 0.0304(17) 0.051(2) -0.0004(15) -0.0016(15) 0.0031(13) C4 0.0413(18) 0.0330(18) 0.0461(19) 0.0015(15) -0.0020(13) 0.0035(13) C1 0.044(2) 0.044(2) 0.053(2) -0.0072(16) 0.0018(15) -0.0013(14) C3 0.0370(19) 0.0301(17) 0.048(2) -0.0004(14) -0.0016(14) -0.0009(13) C6 0.0424(19) 0.041(2) 0.045(2) 0.0055(15) 0.0019(15) 0.0051(15) C5 0.051(2) 0.0333(17) 0.055(2) 0.0072(15) 0.0030(17) 0.0073(16) C8 0.059(2) 0.041(2) 0.0383(17) 0.0006(14) 0.0026(15) 0.0012(17) C9 0.068(3) 0.057(2) 0.0394(19) 0.0001(17) 0.0001(18) 0.004(2) C7 0.081(3) 0.051(3) 0.061(3) 0.016(2) 0.000(2) -0.011(2) C10 0.115(5) 0.092(4) 0.059(3) -0.024(3) -0.015(3) -0.005(4) 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' 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' S S 0.1246 0.1234 '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 C1 S002 C4 90.24(17) . . ? C9 O2 C10 116.7(4) . . ? C1 C2 H2 123.6 . . ? C1 C2 C3 112.9(3) . . ? C3 C2 H2 123.6 . . ? C3 C4 S002 112.9(3) . . ? C3 C4 C5 127.5(3) . . ? C5 C4 S002 119.6(3) . . ? S002 C1 Br1 119.9(2) . . ? C2 C1 Br1 126.8(3) . . ? C2 C1 S002 113.3(3) . . ? C2 C3 C6 123.8(3) . . ? C4 C3 C2 110.7(3) . . ? C4 C3 C6 125.5(3) . . ? C3 C6 C7 115.6(4) . . ? C8 C6 C3 118.2(3) . . ? C8 C6 C7 126.2(3) . . ? N1 C5 C4 178.3(5) . . ? C6 C8 H8 116.8 . . ? C6 C8 C9 126.3(4) . . ? C9 C8 H8 116.8 . . ? O2 C9 C8 109.6(3) . . ? O1 C9 O2 123.5(4) . . ? O1 C9 C8 126.9(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C10 H10A 109.5 . . ? O2 C10 H10B 109.5 . . ? O2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 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 C1 1.862(4) . ? S002 C4 1.722(4) . ? S002 C1 1.707(4) . ? O2 C9 1.329(5) . ? O2 C10 1.441(6) . ? O1 C9 1.201(5) . ? N1 C5 1.127(5) . ? C2 H2 0.9300 . ? C2 C1 1.350(5) . ? C2 C3 1.418(5) . ? C4 C3 1.378(5) . ? C4 C5 1.430(5) . ? C3 C6 1.488(5) . ? C6 C8 1.334(5) . ? C6 C7 1.495(5) . ? C8 H8 0.9300 . ? C8 C9 1.477(5) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ?