#------------------------------------------------------------------------------ #$Date: 2024-09-06 02:45:47 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294468 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572102.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_1572102 loop_ _publ_author_name 'Xie, Kejing' 'Shen, Zeyuan' 'Cheng, Peng' 'Dong, Haoxiang' 'Yu, Zhi-Xiang' 'Zu, Liansuo' _publ_section_title ; C-H functionalization of 2-alkyl tryptamines: direct assembly of azepino[4,5-b]indoles and total synthesis of ngouniensines. ; _journal_issue 32 _journal_name_full 'Chemical science' _journal_page_first 12732 _journal_page_last 12738 _journal_paper_doi 10.1039/d4sc02802c _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C29 H27 Br N2 O3' _chemical_formula_sum 'C29 H27 Br N2 O3' _chemical_formula_weight 531.43 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2022-10-14 _audit_creation_method ; Olex2 1.1 (compiled 2011.02.15 svn.r1672, GUI svn.r3494) ; _audit_update_record ; 2023-07-26 deposited with the CCDC. 2024-07-05 downloaded from the CCDC. ; _cell_angle_alpha 85.389(6) _cell_angle_beta 79.331(9) _cell_angle_gamma 68.354(8) _cell_formula_units_Z 1 _cell_length_a 7.1378(8) _cell_length_b 8.1657(5) _cell_length_c 11.6045(11) _cell_measurement_reflns_used 3830 _cell_measurement_temperature 116.5(3) _cell_measurement_theta_max 71.0150 _cell_measurement_theta_min 3.8750 _cell_volume 617.75(11) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'A short history of SHELX (Sheldrick, 2007)/Bruker' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 116.5(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0971 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.9991 _diffrn_measured_fraction_theta_max 0.8701 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 121.00 147.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 90.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega 104.00 133.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 76.0000 47.0000 78.3566 29 #__ type_ start__ end____ width___ exp.time_ 3 omega 90.00 157.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 61.0000 0.0000 67 #__ type_ start__ end____ width___ exp.time_ 4 omega 139.00 172.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 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40.0000 95.0000 52.5622 25 #__ type_ start__ end____ width___ exp.time_ 61 omega 3.00 28.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 95.0000 73.6372 25 #__ type_ start__ end____ width___ exp.time_ 62 omega -18.00 25.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 40.0000 172.5514 43 #__ type_ start__ end____ width___ exp.time_ 63 omega 4.00 29.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 40.0000 94.0000 -44.5796 25 #__ type_ start__ end____ width___ exp.time_ 64 omega 17.00 42.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 48.0000 84.0000 -44.1874 25 #__ type_ start__ end____ width___ exp.time_ 65 omega 20.00 47.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 35.8017 57.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 66 omega 20.00 63.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 48.0000 79.0000 -157.7796 43 #__ type_ start__ end____ width___ exp.time_ 67 omega 20.00 45.00 1.0000 2.0000 omega____ theta____ kappa____ phi______ frames - 35.8017 57.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 68 omega 51.00 102.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 108.0000 -94.0000 -180.0000 51 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.1052976000 _diffrn_orient_matrix_UB_12 0.2010240000 _diffrn_orient_matrix_UB_13 0.0140305000 _diffrn_orient_matrix_UB_21 0.1059645000 _diffrn_orient_matrix_UB_22 0.0277764000 _diffrn_orient_matrix_UB_23 -0.1242559000 _diffrn_orient_matrix_UB_31 -0.1821280000 _diffrn_orient_matrix_UB_32 -0.0052056000 _diffrn_orient_matrix_UB_33 -0.0511489000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0530 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 8110 _diffrn_reflns_point_group_measured_fraction_full 0.894 _diffrn_reflns_point_group_measured_fraction_max 0.869 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.107 _diffrn_reflns_theta_min 3.877 _diffrn_source 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.539 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.429 _exptl_crystal_F_000 274 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.015 _refine_diff_density_max 0.543 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.055 _refine_ls_abs_structure_details ; Flack x determined using 1606 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.017(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4161 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0367 _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^)+(0.0405P)^2^+0.1794P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.0911 _reflns_Friedel_coverage 0.771 _reflns_Friedel_fraction_full 0.790 _reflns_Friedel_fraction_max 0.757 _reflns_number_gt 3970 _reflns_number_total 4161 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02802c2.cif _cod_data_source_block exp_8216 _cod_depositor_comments 'Adding full bibliography for 1572101--1572103.cif.' _cod_database_code 1572102 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _shelx_estimated_absorpt_t_max 0.963 _shelx_estimated_absorpt_t_min 0.470 _shelx_hkl_checksum 42142 _shelx_hkl_file ; -8 -6 -6 1039.03 256.566 68 -8 -6 -5 838.764 290.946 68 -8 -6 -4 1091.93 303.997 68 -8 -6 -3 1953.73 389.935 68 -8 -6 -2 7513.06 626.648 52 -8 -6 -1 5479.42 539.763 52 -8 -6 0 524.150 149.721 52 -8 -5 -6 2207.78 383.725 68 -8 -5 -5 805.077 253.256 52 -8 -5 -5 822.284 290.619 68 -8 -5 -4 2329.45 418.861 52 -8 -5 -4 2648.45 483.730 68 -8 -5 -3 261.402 201.529 52 -8 -5 -2 2728.85 457.903 52 -8 -5 -1 943.153 275.495 52 -8 -5 0 102.427 170.332 52 -8 -5 1 6992.94 653.322 52 -8 -5 2 2844.08 406.389 52 -8 -4 -7 2383.33 393.088 52 -8 -4 -6 2342.27 420.300 52 -8 -4 -5 402.090 258.949 52 -8 -4 -4 826.042 301.136 52 -8 -4 -3 3745.64 565.588 52 -8 -4 -2 8139.63 837.809 52 -8 -4 -1 1641.21 370.244 52 -8 -4 0 197.094 229.240 52 -8 -4 1 2631.83 445.348 52 -8 -4 2 4293.11 526.046 52 -8 -4 3 7836.66 621.867 52 -8 -3 -7 5360.49 598.493 52 -8 -3 -6 7451.50 746.866 52 -8 -3 -5 7332.80 782.122 52 -8 -3 -4 2348.19 477.189 52 -8 -3 -3 148.641 219.112 52 -8 -3 -2 7379.39 786.229 52 -8 -3 -1 2535.37 487.371 52 -8 -3 0 3513.88 527.329 52 -8 -3 1 6043.88 588.610 47 -8 -3 1 5906.88 649.130 52 -8 -3 2-189.157 158.111 47 -8 -3 2 201.284 172.493 52 -8 -2 -7 1175.17 301.370 52 -8 -2 -6 15653.3 1071.22 52 -8 -2 -5 2092.82 444.016 52 -8 -2 -4 7418.95 782.536 52 -8 -2 -3 1458.62 388.615 52 -8 -2 -2 6016.58 682.398 52 -8 -2 -1-130.187 202.346 52 -8 -2 0 1567.35 356.015 52 -8 -2 0 1491.92 342.821 47 -8 -2 1 1383.43 319.080 52 -8 -2 1 1248.35 306.813 47 -8 -2 2 4939.98 530.144 47 -8 -2 2 4509.62 475.857 52 -8 -1 -6 4448.19 535.526 52 -8 -1 -5 1607.27 353.775 52 -8 -1 -4 146.892 185.701 52 -8 -1 -3 4240.95 566.158 52 -8 -1 -2 5320.30 555.526 47 -8 -1 -2 3939.34 526.713 52 -8 -1 -1 2408.34 414.392 47 -8 -1 -1 3071.71 441.643 52 -8 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895.164 373.905 7 5 4 -6 287.872 382.444 12 5 4 -5 3538.89 686.483 12 5 4 -4 5732.65 1641.39 33 5 4 -4 5687.05 891.988 31 5 4 -3 3847.00 1329.85 33 5 4 -3 4075.34 742.948 31 5 4 -2 65187.0 5202.64 33 5 4 -2 68671.8 2993.39 31 5 4 -1 845.853 711.788 33 5 4 -1 43.1654 244.591 31 5 4 0 39649.0 3865.29 33 5 4 0 36780.3 2040.18 31 5 4 1 9262.09 1726.40 65 5 4 1 9085.49 1862.26 33 5 4 1 10466.7 1683.37 32 5 4 2 2531.60 778.753 66 5 4 2 5000.38 1222.94 32 5 4 3-834.122 579.503 66 5 4 3-291.295 437.250 32 5 4 4 21557.0 2545.74 66 5 4 4 19336.4 2388.17 45 5 4 4 19605.5 2478.61 32 5 4 5 9308.07 1771.91 66 5 4 5 4216.27 1195.60 45 5 4 6 27821.8 3136.36 66 5 4 7 13381.3 2053.53 44 5 5 -9 4046.73 461.826 12 5 5 -9 2869.24 412.399 11 5 5 -8 6427.63 716.167 12 5 5 -8 6881.92 752.416 11 5 5 -7 283.219 244.290 12 5 5 -7 537.395 247.758 16 5 5 -6 3609.80 662.327 7 5 5 -6 2422.47 567.527 12 5 5 -5 3458.70 692.720 12 5 5 -5 5355.71 860.326 31 5 5 -4 2674.35 635.566 31 5 5 -3 3758.39 1315.40 33 5 5 -3 6842.08 972.158 31 5 5 -2 31017.2 3658.95 33 5 5 -2 31443.7 2074.63 31 5 5 -1 51737.3 4620.40 33 5 5 -1 47945.9 2551.38 31 5 5 0 27261.9 3297.61 33 5 5 0 33089.0 2052.80 31 5 5 1 7003.23 1480.01 66 5 5 1 8151.06 1826.81 33 5 5 1 6632.62 1527.90 32 5 5 2 5275.45 1345.02 66 5 5 2 7125.53 1542.40 32 5 5 3 10485.8 1880.39 66 5 5 3 8217.81 1731.95 32 5 5 4 42703.1 3806.50 66 5 5 4 43211.7 3905.38 32 5 5 5 16898.0 2469.55 66 5 5 5 16004.7 2438.84 32 5 6 -8 1194.91 297.791 12 5 6 -8 1211.19 310.106 11 5 6 -7 1808.21 445.427 12 5 6 -6 947.280 385.344 12 5 6 -6 1984.52 402.892 29 5 6 -5 6975.92 925.969 12 5 6 -5 7414.09 831.953 29 5 6 -4 6079.95 922.478 31 5 6 -4 5139.16 740.045 29 5 6 -3 123.135 267.830 31 5 6 -3 329.019 327.525 29 5 6 -2 4837.59 869.849 31 5 6 -1 7031.58 1000.42 31 5 6 0 12973.8 2482.07 33 5 6 0 18463.7 1613.07 31 5 6 1 3842.22 1262.03 33 5 6 2 10272.2 2010.80 32 5 6 3 5621.01 1605.35 32 5 7 -7 242.061 197.054 12 5 7 -6 2684.38 503.762 12 5 7 -6 2973.01 449.499 29 5 7 -5 256.415 272.524 12 5 7 -5 456.934 187.171 29 5 7 -4 15398.0 1234.43 29 5 7 -3 1495.07 532.226 31 5 7 -3 584.986 214.505 29 5 7 -2 4204.69 815.771 31 5 7 -2 4871.53 760.010 29 5 7 -1 12549.7 1367.68 31 5 7 0 559.577 381.072 31 5 7 1-62.3561 351.798 31 5 8 -5 3051.28 456.407 12 5 8 -5 3461.30 472.592 29 5 8 -4 777.179 290.394 12 5 8 -4 1165.19 344.089 29 5 8 -3 308.981 245.014 29 5 8 -2 1591.59 467.231 29 5 8 -1 2792.20 594.485 29 5 8 1 3408.10 590.625 30 5 8 2 20845.0 1460.33 30 5 9 -3 3576.68 479.010 29 5 9 -2 1524.05 369.546 29 5 9 -1 517.379 264.856 29 5 9 0 5427.90 689.667 29 5 9 1 685.167 240.632 30 5 9 2 509.570 228.045 30 5 9 3 1798.46 401.083 30 5 9 4 598.371 279.573 30 5 9 5 3925.02 537.262 30 5 9 6 621.460 243.910 30 6 -4 -1 4968.04 464.859 14 6 -4 0 11210.8 723.238 14 6 -4 1 1479.86 269.236 14 6 -4 4 2927.46 371.636 13 6 -3 -4 3368.68 403.714 8 6 -3 -3 130.003 167.516 14 6 -3 -3 167.789 164.644 8 6 -3 -3 338.572 206.988 15 6 -3 -2 10993.5 846.742 14 6 -3 -2 10323.6 822.894 8 6 -3 -2 10486.0 750.399 15 6 -3 0-403.553 195.263 8 6 -3 2 6023.05 652.801 14 6 -3 3 96.1477 138.251 14 6 -2 -5 1180.22 252.845 14 6 -2 -5 1602.36 330.472 15 6 -2 -4 3541.88 517.153 15 6 -2 -3 2418.74 462.677 15 6 -2 -2 4557.01 635.262 20 6 -2 -2 5933.78 723.596 15 6 -2 -1 1101.03 361.922 20 6 -2 -1 146.163 183.684 15 6 -1 -6 549.573 231.645 15 6 -1 -5 2263.77 456.864 15 6 -1 -4 6614.84 776.449 20 6 -1 -3 3803.60 630.343 20 6 -1 -2 1078.52 360.990 20 6 -1 -1 18690.7 1389.12 20 6 -1 0 22315.4 1479.38 20 6 0 -7 23.6224 151.059 16 6 0 -7 436.909 181.281 15 6 0 -6 18690.4 1178.96 16 6 0 -6 15694.8 1101.23 15 6 0 -5 7282.80 824.214 20 6 0 -5 7360.94 825.456 16 6 0 -4 5792.00 787.234 20 6 0 -4 4917.97 718.134 16 6 0 0 6336.53 820.109 20 6 1 -8 4010.83 457.885 16 6 1 -7 1010.01 317.072 16 6 1 -7 992.517 281.705 15 6 1 -6 5432.20 728.605 16 6 1 -5 185.871 289.861 16 6 1 -4 1414.26 472.935 16 6 1 0 9817.18 2063.14 34 6 1 1 15617.9 2641.63 34 6 1 2 11880.1 2297.45 34 6 1 3 10402.8 2064.14 34 6 1 4 1318.18 864.105 34 6 2 -8 1104.61 288.597 16 6 2 -7 2002.08 399.861 11 6 2 -7 1790.45 411.806 16 6 2 -6 2438.04 492.471 11 6 2 -6 2349.56 540.780 16 6 2 -5 266.544 211.553 11 6 2 -1 1534.80 953.788 33 6 2 1-735.979 799.816 64 6 2 2 3765.54 1351.42 64 6 2 3 28574.3 3301.45 64 6 2 4 36673.5 3762.34 34 6 3 -8 864.661 257.431 11 6 3 -8 1112.89 282.221 16 6 3 -7 853.194 304.278 11 6 3 -7 961.884 350.926 16 6 3 -6 4765.50 623.186 12 6 3 -6 5468.47 726.341 11 6 3 -6 4056.13 671.881 16 6 3 -5 442.994 210.665 11 6 3 -4 218.653 267.076 11 6 3 -1 1326.01 858.033 33 6 3 0 6591.54 1603.30 64 6 3 0 3486.08 1261.51 33 6 3 1 7603.44 1737.86 33 6 3 2 21017.6 2897.05 33 6 3 3 43781.7 4165.22 33 6 4 -8 499.438 186.928 11 6 4 -7 7607.74 717.988 12 6 4 -7 7906.93 764.624 11 6 4 -7 6456.70 712.296 16 6 4 -6 2424.09 473.902 12 6 4 -6 2181.24 476.278 11 6 4 -5 263.556 222.979 12 6 4 -4 798.750 372.306 12 6 4 -2 23015.4 1697.97 31 6 4 -1 16560.0 1423.74 31 6 4 0 11802.7 2364.05 33 6 4 0 18911.2 1498.08 31 6 4 1 24841.8 3198.95 33 6 4 1 24827.4 1719.48 31 6 4 2 15162.1 2508.78 33 6 4 2 15338.3 1340.05 31 6 4 3 6899.98 1715.20 33 6 4 4 1155.57 802.232 33 6 5 -7 224.819 163.583 12 6 5 -7 375.296 197.255 11 6 5 -7 177.643 178.204 16 6 5 -6 2354.57 479.884 12 6 5 -5 300.090 273.948 12 6 5 -4 6793.71 883.076 12 6 5 -3 6225.34 914.589 31 6 5 -2 12316.5 1292.81 31 6 5 -1 4702.59 785.473 31 6 5 0 14429.5 1374.34 31 6 5 1 4485.93 760.055 31 6 6 -6 1685.25 379.015 12 6 6 -6 868.675 284.242 16 6 6 -5 375.880 258.870 12 6 6 -4 5015.40 752.367 12 6 6 -2 26124.0 1871.51 31 6 6 -1 4869.79 821.956 31 6 6 0 1803.31 550.648 31 6 6 1 5978.56 934.223 31 6 6 2 529.335 302.054 31 6 7 -5-127.872 181.303 12 6 7 -4 370.074 248.979 12 6 7 -3 529.476 212.109 29 6 7 -2 4732.15 648.245 29 6 7 -1 1773.21 446.607 29 6 7 0 1398.56 524.514 31 6 7 1-199.120 291.498 31 6 7 2 4372.78 790.118 31 6 7 3 843.708 409.633 31 6 8 -3 20.0945 213.781 12 6 8 -3-657.458 225.158 29 6 8 -2 3484.07 527.628 29 6 8 -1 7997.45 821.510 29 6 9 0 8246.28 728.175 29 6 9 1 9486.73 810.340 29 7 -1 -3 4534.89 502.758 15 7 -1 -2 4163.91 511.064 15 7 -1 -1 1065.72 277.744 15 7 0 -5 3018.52 391.316 15 7 0 -4 4121.91 517.417 15 7 1 -5 695.350 213.432 16 7 1 -4 3357.32 471.612 16 7 1 -2 7288.81 825.704 20 7 1 -1 6903.86 797.192 20 7 2 -6 2629.97 378.309 16 7 2 -5 2177.82 412.158 16 7 2 -4 1398.80 402.316 16 7 2 -3 456.080 299.638 16 7 3 -6 1105.09 290.104 16 7 3 -5 3053.46 512.636 16 7 4 -6 707.192 222.215 16 7 4 -5 2922.60 500.028 16 7 5 -5 14554.0 992.666 16 7 5 -4 2502.37 435.391 12 7 5 -3 314.400 229.561 12 7 6 -4 2652.66 422.252 12 7 6 -3 4249.35 583.115 12 7 7 -3 1110.56 314.319 12 7 8 1 868.388 239.243 29 8 3 -2 420.461 229.550 16 0 0 0 0.00 0.00 0 TITL exp_8216 in P1 REM P1 (#1 in standard setting) CELL 1.54184 7.136681 8.165018 11.603653 85.3962 79.3546 68.3615 ZERR 3.00 0.000457 0.000378 0.000637 0.0041 0.0050 0.0051 LATT -1 SFAC C H N O UNIT 33.00 30.00 3.00 3.00 TREF HKLF 4 END ; _shelx_res_checksum 95424 _shelx_res_file ; exp_8216.res created by SHELXL-2014/7 TITL exp_8216 in P1 #1 CELL 1.54184 7.13778 8.16572 11.60451 85.3887 79.331 68.354 ZERR 1 0.00084 0.00054 0.00105 0.0063 0.0087 0.0083 LATT -1 SFAC C H Br N O UNIT 29 27 1 2 3 L.S. 3 PLAN 15 SIZE 0.015 0.35 0.06 REM reset to P1 #1 bond $H conf htab fmap 2 acta REM D:/zuliansuo/exp_8216/struct/olex2_exp_8216/exp_8216.hkl WGHT 0.040500 0.179400 FVAR 9.64083 BR1 3 -0.639140 -0.477550 -0.058350 11.00000 0.05698 0.05279 = 0.02666 -0.00759 -0.01747 -0.00687 O1 5 -0.447004 -0.460221 0.483016 11.00000 0.02516 0.01506 = 0.02141 -0.00460 -0.00125 -0.00481 C3 1 -0.420632 -0.900858 0.637000 11.00000 0.01804 0.01798 = 0.01281 0.00070 0.00036 -0.00683 O3 5 -0.189367 -0.526263 0.709208 11.00000 0.03165 0.02020 = 0.02162 -0.00243 -0.00212 -0.01296 N1 4 -0.429044 -1.138746 0.555814 11.00000 0.02154 0.01380 = 0.01675 -0.00480 -0.00116 -0.00530 AFIX 43 H1 2 -0.395759 -1.226633 0.510264 11.00000 -1.20000 AFIX 0 O2 5 -0.022350 -0.517168 0.526472 11.00000 0.02766 0.02743 = 0.02761 -0.00320 0.00097 -0.01522 N2 4 -0.213254 -0.735879 0.458184 11.00000 0.01924 0.01518 = 0.01680 -0.00236 0.00232 -0.00612 C6 1 -0.113651 -0.900882 0.391930 11.00000 0.01900 0.01388 = 0.01577 -0.00282 0.00126 -0.00588 AFIX 13 H6 2 -0.188904 -0.893227 0.327883 11.00000 -1.20000 AFIX 0 C4 1 -0.320760 -1.027864 0.553163 11.00000 0.02145 0.01331 = 0.01568 0.00142 -0.00258 -0.00501 C7 1 -0.599558 -0.934659 0.693951 11.00000 0.02185 0.01536 = 0.01698 0.00342 -0.00809 -0.00741 C9 1 -0.747209 -1.159371 0.679868 11.00000 0.02181 0.01766 = 0.01990 -0.00052 -0.00617 -0.00915 AFIX 43 H9 2 -0.743171 -1.260242 0.645924 11.00000 -1.20000 AFIX 0 C12 1 -0.757839 -0.853273 0.785390 11.00000 0.02182 0.01800 = 0.01590 0.00077 -0.00659 -0.00569 AFIX 43 H12 2 -0.761617 -0.753807 0.821004 11.00000 -1.20000 AFIX 0 C13 1 0.106157 -0.923060 0.337750 11.00000 0.02401 0.01731 = 0.01951 -0.00409 0.00387 -0.00891 AFIX 23 H13A 2 0.188794 -0.951173 0.399321 11.00000 -1.20000 H13B 2 0.108502 -0.812514 0.301335 11.00000 -1.20000 AFIX 0 C21 1 -0.123362 -0.578792 0.598677 11.00000 0.01697 0.01716 = 0.02127 -0.00082 -0.00316 -0.00456 C10 1 -0.902365 -1.074834 0.769988 11.00000 0.01834 0.02461 = 0.02232 0.00272 -0.00214 -0.01104 AFIX 43 H10 2 -1.004968 -1.119979 0.796648 11.00000 -1.20000 AFIX 0 C14 1 0.199980 -1.068807 0.245589 11.00000 0.02357 0.02571 = 0.03117 -0.01371 0.00485 -0.01007 AFIX 23 H14A 2 0.210215 -1.181031 0.284013 11.00000 -1.20000 H14B 2 0.108891 -1.047142 0.188939 11.00000 -1.20000 AFIX 0 C5 1 -0.122742 -1.061181 0.470631 11.00000 0.01907 0.01666 = 0.02103 -0.00343 0.00140 -0.00543 AFIX 23 H5A 2 -0.099613 -1.158894 0.420732 11.00000 -1.20000 H5B 2 -0.012568 -1.096179 0.516021 11.00000 -1.20000 AFIX 0 C23 1 -0.357714 -0.591776 0.421179 11.00000 0.01946 0.01602 = 0.01764 -0.00212 0.00213 -0.00841 C17 1 0.770741 -1.169248 0.176075 11.00000 0.02321 0.03193 = 0.03269 -0.00422 -0.00660 -0.00897 AFIX 43 H17 2 0.883874 -1.219025 0.213474 11.00000 -1.20000 AFIX 0 C25 1 -0.276966 -0.591811 0.199103 11.00000 0.02564 0.02900 = 0.02426 -0.00337 -0.00111 -0.00646 AFIX 43 H25 2 -0.140478 -0.613975 0.202178 11.00000 -1.20000 AFIX 0 C8 1 -0.597569 -1.086457 0.642410 11.00000 0.02075 0.01629 = 0.01432 0.00029 -0.00300 -0.00347 C16 1 0.576994 -1.153921 0.235888 11.00000 0.03080 0.02619 = 0.01926 -0.00141 -0.00047 -0.00972 AFIX 43 H16 2 0.561844 -1.193262 0.313287 11.00000 -1.20000 AFIX 0 C2 1 -0.360467 -0.753231 0.666953 11.00000 0.02198 0.01780 = 0.01821 -0.00151 -0.00113 -0.00883 AFIX 23 H2A 2 -0.324549 -0.774030 0.744859 11.00000 -1.20000 H2B 2 -0.476580 -0.643389 0.668160 11.00000 -1.20000 AFIX 0 C24 1 -0.413474 -0.589622 0.301827 11.00000 0.02103 0.01342 = 0.02049 -0.00278 -0.00060 -0.00434 C1 1 -0.178821 -0.735679 0.579069 11.00000 0.01955 0.01684 = 0.01879 -0.00018 -0.00124 -0.00839 AFIX 13 H1A 2 -0.059638 -0.841512 0.588712 11.00000 -1.20000 AFIX 0 C26 1 -0.345013 -0.560696 0.091316 11.00000 0.03654 0.03506 = 0.02005 -0.00415 0.00143 -0.00922 AFIX 43 H26 2 -0.255393 -0.558086 0.022542 11.00000 -1.20000 AFIX 0 C19 1 0.625728 -1.036410 0.007240 11.00000 0.03867 0.05534 = 0.02211 0.00789 0.00461 -0.01484 AFIX 43 H19 2 0.640361 -0.994711 -0.069600 11.00000 -1.20000 AFIX 0 C27 1 -0.545442 -0.533960 0.087646 11.00000 0.03798 0.02167 = 0.02154 -0.00551 -0.01474 -0.00118 C18 1 0.794880 -1.110642 0.061425 11.00000 0.02163 0.04160 = 0.03276 -0.00669 0.00779 -0.01458 AFIX 43 H18 2 0.924026 -1.121103 0.021063 11.00000 -1.20000 AFIX 0 C15 1 0.407238 -1.081164 0.181861 11.00000 0.02547 0.02129 = 0.01914 -0.00735 0.00044 -0.01087 C11 1 -0.909236 -0.923945 0.821939 11.00000 0.02139 0.02517 = 0.01725 -0.00240 0.00079 -0.00667 AFIX 43 H11 2 -1.016429 -0.870031 0.881745 11.00000 -1.20000 AFIX 0 C29 1 -0.616421 -0.563411 0.295839 11.00000 0.02435 0.02217 = 0.02206 -0.00284 0.00005 -0.00855 AFIX 43 H29 2 -0.707938 -0.563816 0.364172 11.00000 -1.20000 AFIX 0 C28 1 -0.681306 -0.536795 0.187955 11.00000 0.02384 0.02897 = 0.03574 -0.00581 -0.00747 -0.00823 AFIX 43 H28 2 -0.815669 -0.520994 0.183542 11.00000 -1.20000 AFIX 0 C22 1 -0.124944 -0.393708 0.745296 11.00000 0.04559 0.02565 = 0.02871 -0.00174 -0.00922 -0.01929 AFIX 137 H22A 2 -0.191239 -0.283318 0.708059 11.00000 -1.50000 H22B 2 0.020560 -0.427964 0.723022 11.00000 -1.50000 H22C 2 -0.161166 -0.381392 0.828889 11.00000 -1.50000 AFIX 0 C20 1 0.434779 -1.023801 0.066681 11.00000 0.02805 0.04691 = 0.02489 0.00198 -0.00415 -0.00598 AFIX 43 H20 2 0.322337 -0.975787 0.028567 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_8216 in P1 #1 REM R1 = 0.0367 for 3970 Fo > 4sig(Fo) and 0.0390 for all 4161 data REM 317 parameters refined using 3 restraints END WGHT 0.0405 0.1794 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB N1 O1_$1 HTAB C2 O1 EQIV $2 x, y+1, z HTAB C22 N1_$2 REM Highest difference peak 0.543, deepest hole -0.285, 1-sigma level 0.055 Q1 1 -0.7364 -0.5040 -0.0099 11.00000 0.05 0.54 Q2 1 -0.5737 -0.5622 -0.1183 11.00000 0.05 0.30 Q3 1 -0.5950 -0.4954 0.1592 11.00000 0.05 0.28 Q4 1 -0.6642 -0.4310 0.0243 11.00000 0.05 0.27 Q5 1 -0.3381 -0.5604 0.2652 11.00000 0.05 0.24 Q6 1 0.1298 -0.9838 0.2972 11.00000 0.05 0.23 Q7 1 -0.2439 -1.0208 0.5046 11.00000 0.05 0.22 Q8 1 -0.5206 -0.4380 -0.1172 11.00000 0.05 0.20 Q9 1 0.0822 -0.5812 0.4691 11.00000 0.05 0.20 Q10 1 -0.2763 -0.7245 0.6305 11.00000 0.05 0.19 Q11 1 -0.4837 -0.3940 0.2739 11.00000 0.05 0.19 Q12 1 0.1393 -1.1423 0.2342 11.00000 0.05 0.19 Q13 1 -0.1306 -0.9809 0.4358 11.00000 0.05 0.19 Q14 1 -0.5447 -0.8828 0.6553 11.00000 0.05 0.19 Q15 1 -0.8763 -1.0864 0.6810 11.00000 0.05 0.19 ; _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.63914(6) -0.47755(5) -0.05835(5) 0.0474(2) Uani 1 1 d . . . . . O1 O -0.4470(5) -0.4602(4) 0.4830(3) 0.0214(7) Uani 1 1 d . . . . . C3 C -0.4206(7) -0.9009(5) 0.6370(4) 0.0166(9) Uani 1 1 d . . . . . O3 O -0.1894(5) -0.5263(4) 0.7092(3) 0.0237(7) Uani 1 1 d . . . . . N1 N -0.4290(6) -1.1387(4) 0.5558(3) 0.0177(7) Uani 1 1 d . . . . . H1 H -0.3958 -1.2266 0.5103 0.021 Uiso 1 1 calc R U . . . O2 O -0.0224(5) -0.5172(4) 0.5265(3) 0.0267(7) Uani 1 1 d . . . . . N2 N -0.2133(6) -0.7359(4) 0.4582(3) 0.0177(7) Uani 1 1 d . . . . . C6 C -0.1137(7) -0.9009(5) 0.3919(4) 0.0167(9) Uani 1 1 d . . . . . H6 H -0.1889 -0.8932 0.3279 0.020 Uiso 1 1 calc R U . . . C4 C -0.3208(7) -1.0279(5) 0.5532(4) 0.0173(9) Uani 1 1 d . . . . . C7 C -0.5996(7) -0.9347(5) 0.6940(4) 0.0174(9) Uani 1 1 d . . . . . C9 C -0.7472(7) -1.1594(5) 0.6799(4) 0.0188(9) Uani 1 1 d . . . . . H9 H -0.7432 -1.2602 0.6459 0.023 Uiso 1 1 calc R U . . . C12 C -0.7578(7) -0.8533(5) 0.7854(4) 0.0186(9) Uani 1 1 d . . . . . H12 H -0.7616 -0.7538 0.8210 0.022 Uiso 1 1 calc R U . . . C13 C 0.1062(8) -0.9231(6) 0.3378(4) 0.0207(10) Uani 1 1 d . . . . . H13A H 0.1888 -0.9512 0.3993 0.025 Uiso 1 1 calc R U . . . H13B H 0.1085 -0.8125 0.3013 0.025 Uiso 1 1 calc R U . . . C21 C -0.1234(7) -0.5788(5) 0.5987(4) 0.0189(9) Uani 1 1 d . . . . . C10 C -0.9024(7) -1.0748(6) 0.7700(4) 0.0212(9) Uani 1 1 d . . . . . H10 H -1.0050 -1.1200 0.7966 0.025 Uiso 1 1 calc R U . . . C14 C 0.2000(8) -1.0688(6) 0.2456(5) 0.0270(11) Uani 1 1 d . . . . . H14A H 0.2102 -1.1810 0.2840 0.032 Uiso 1 1 calc R U . . . H14B H 0.1089 -1.0471 0.1889 0.032 Uiso 1 1 calc R U . . . C5 C -0.1227(7) -1.0612(6) 0.4706(4) 0.0197(10) Uani 1 1 d . . . . . H5A H -0.0996 -1.1589 0.4207 0.024 Uiso 1 1 calc R U . . . H5B H -0.0126 -1.0962 0.5160 0.024 Uiso 1 1 calc R U . . . C23 C -0.3577(7) -0.5918(5) 0.4212(4) 0.0177(8) Uani 1 1 d . . . . . C17 C 0.7707(8) -1.1692(6) 0.1761(4) 0.0291(10) Uani 1 1 d . . . . . H17 H 0.8839 -1.2190 0.2135 0.035 Uiso 1 1 calc R U . . . C25 C -0.2770(8) -0.5918(6) 0.1991(4) 0.0275(11) Uani 1 1 d . . . . . H25 H -0.1405 -0.6140 0.2022 0.033 Uiso 1 1 calc R U . . . C8 C -0.5976(7) -1.0865(5) 0.6424(3) 0.0181(9) Uani 1 1 d . . . . . C16 C 0.5770(8) -1.1539(6) 0.2359(4) 0.0260(10) Uani 1 1 d . . . . . H16 H 0.5618 -1.1933 0.3133 0.031 Uiso 1 1 calc R U . . . C2 C -0.3605(7) -0.7532(5) 0.6670(4) 0.0191(9) Uani 1 1 d . . . . . H2A H -0.3245 -0.7740 0.7449 0.023 Uiso 1 1 calc R U . . . H2B H -0.4766 -0.6434 0.6682 0.023 Uiso 1 1 calc R U . . . C24 C -0.4135(7) -0.5896(5) 0.3018(4) 0.0191(9) Uani 1 1 d . . . . . C1 C -0.1788(7) -0.7357(5) 0.5791(4) 0.0181(9) Uani 1 1 d . . . . . H1A H -0.0596 -0.8415 0.5887 0.022 Uiso 1 1 calc R U . . . C26 C -0.3450(9) -0.5607(7) 0.0913(4) 0.0322(12) Uani 1 1 d . . . . . H26 H -0.2554 -0.5581 0.0225 0.039 Uiso 1 1 calc R U . . . C19 C 0.6257(10) -1.0364(8) 0.0072(5) 0.0411(15) Uani 1 1 d . . . . . H19 H 0.6404 -0.9947 -0.0696 0.049 Uiso 1 1 calc R U . . . C27 C -0.5454(8) -0.5340(6) 0.0876(4) 0.0282(11) Uani 1 1 d . . . . . C18 C 0.7949(8) -1.1106(7) 0.0614(4) 0.0324(12) Uani 1 1 d . . . . . H18 H 0.9240 -1.1211 0.0211 0.039 Uiso 1 1 calc R U . . . C15 C 0.4072(7) -1.0812(6) 0.1819(4) 0.0214(10) Uani 1 1 d . . . . . C11 C -0.9092(7) -0.9239(6) 0.8219(4) 0.0222(10) Uani 1 1 d . . . . . H11 H -1.0164 -0.8700 0.8817 0.027 Uiso 1 1 calc R U . . . C29 C -0.6164(7) -0.5634(6) 0.2958(4) 0.0232(10) Uani 1 1 d . . . . . H29 H -0.7079 -0.5638 0.3642 0.028 Uiso 1 1 calc R U . . . C28 C -0.6813(8) -0.5368(6) 0.1880(4) 0.0292(11) Uani 1 1 d . . . . . H28 H -0.8157 -0.5210 0.1835 0.035 Uiso 1 1 calc R U . . . C22 C -0.1249(9) -0.3937(6) 0.7453(4) 0.0310(11) Uani 1 1 d . . . . . H22A H -0.1912 -0.2833 0.7081 0.046 Uiso 1 1 calc R U . . . H22B H 0.0206 -0.4280 0.7230 0.046 Uiso 1 1 calc R U . . . H22C H -0.1612 -0.3814 0.8289 0.046 Uiso 1 1 calc R U . . . C20 C 0.4348(9) -1.0238(8) 0.0667(5) 0.0357(13) Uani 1 1 d . . . . . H20 H 0.3223 -0.9758 0.0286 0.043 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 0.0570(4) 0.0528(3) 0.0267(3) -0.0076(2) -0.0175(2) -0.0069(3) O1 0.0252(17) 0.0151(13) 0.0214(15) -0.0046(11) -0.0012(13) -0.0048(12) C3 0.018(2) 0.0180(18) 0.0128(19) 0.0007(15) 0.0004(16) -0.0068(16) O3 0.0317(19) 0.0202(14) 0.0216(15) -0.0024(12) -0.0021(13) -0.0130(14) N1 0.022(2) 0.0138(15) 0.0167(17) -0.0048(13) -0.0012(14) -0.0053(14) O2 0.0277(19) 0.0274(15) 0.0276(16) -0.0032(13) 0.0010(14) -0.0152(14) N2 0.0192(19) 0.0152(15) 0.0168(17) -0.0024(13) 0.0023(14) -0.0061(14) C6 0.019(2) 0.0139(18) 0.016(2) -0.0028(15) 0.0013(17) -0.0059(16) C4 0.021(2) 0.0133(17) 0.016(2) 0.0014(15) -0.0026(17) -0.0050(16) C7 0.022(2) 0.0154(18) 0.017(2) 0.0034(16) -0.0081(17) -0.0074(17) C9 0.022(2) 0.0177(18) 0.020(2) -0.0005(15) -0.0062(17) -0.0091(17) C12 0.022(2) 0.0180(19) 0.016(2) 0.0008(16) -0.0066(17) -0.0057(17) C13 0.024(2) 0.0173(18) 0.020(2) -0.0041(16) 0.0039(18) -0.0089(17) C21 0.017(2) 0.0172(18) 0.021(2) -0.0008(15) -0.0032(17) -0.0046(16) C10 0.018(2) 0.025(2) 0.022(2) 0.0027(17) -0.0021(18) -0.0110(18) C14 0.024(3) 0.026(2) 0.031(3) -0.014(2) 0.005(2) -0.0101(19) C5 0.019(2) 0.0167(19) 0.021(2) -0.0034(16) 0.0014(19) -0.0054(17) C23 0.019(2) 0.0160(18) 0.0176(19) -0.0021(14) 0.0021(16) -0.0084(16) C17 0.023(3) 0.032(2) 0.033(3) -0.0042(19) -0.007(2) -0.009(2) C25 0.026(3) 0.029(2) 0.024(2) -0.0034(19) -0.001(2) -0.006(2) C8 0.021(2) 0.0163(18) 0.0143(18) 0.0003(14) -0.0030(16) -0.0035(16) C16 0.031(3) 0.026(2) 0.019(2) -0.0014(16) -0.0005(19) -0.0097(19) C2 0.022(2) 0.0178(17) 0.018(2) -0.0015(16) -0.0011(17) -0.0088(16) C24 0.021(2) 0.0134(17) 0.020(2) -0.0028(15) -0.0006(18) -0.0043(16) C1 0.020(2) 0.0168(18) 0.019(2) -0.0002(15) -0.0012(17) -0.0084(16) C26 0.037(3) 0.035(2) 0.020(2) -0.0042(19) 0.001(2) -0.009(2) C19 0.039(3) 0.055(3) 0.022(3) 0.008(2) 0.005(2) -0.015(3) C27 0.038(3) 0.022(2) 0.022(2) -0.0055(17) -0.015(2) -0.001(2) C18 0.022(3) 0.042(3) 0.033(3) -0.007(2) 0.008(2) -0.015(2) C15 0.025(3) 0.021(2) 0.019(2) -0.0074(16) 0.0004(19) -0.0109(18) C11 0.021(2) 0.025(2) 0.017(2) -0.0024(17) 0.0008(19) -0.0067(18) C29 0.024(2) 0.022(2) 0.022(2) -0.0028(16) 0.0001(18) -0.0086(18) C28 0.024(3) 0.029(2) 0.036(3) -0.0058(19) -0.007(2) -0.0082(19) C22 0.046(3) 0.026(2) 0.029(2) -0.0017(18) -0.009(2) -0.019(2) C20 0.028(3) 0.047(3) 0.025(3) 0.002(2) -0.004(2) -0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C3 C7 106.7(4) . . ? C4 C3 C2 128.4(4) . . ? C7 C3 C2 124.9(4) . . ? C21 O3 C22 117.0(4) . . ? C4 N1 H1 125.3 . . ? C8 N1 H1 125.3 . . ? C8 N1 C4 109.4(3) . . ? C23 N2 C6 123.7(4) . . ? C23 N2 C1 117.1(3) . . ? C1 N2 C6 118.4(3) . . ? N2 C6 H6 107.9 . . ? N2 C6 C13 110.5(4) . . ? N2 C6 C5 110.9(3) . . ? C13 C6 H6 107.9 . . ? C13 C6 C5 111.5(3) . . ? C5 C6 H6 107.9 . . ? C3 C4 N1 109.2(4) . . ? C3 C4 C5 130.2(4) . . ? N1 C4 C5 120.6(4) . . ? C12 C7 C3 133.6(4) . . ? C12 C7 C8 119.2(4) . . ? C8 C7 C3 107.2(4) . . ? C10 C9 H9 121.5 . . ? C10 C9 C8 117.0(4) . . ? C8 C9 H9 121.5 . . ? C7 C12 H12 120.6 . . ? C11 C12 C7 118.7(4) . . ? C11 C12 H12 120.6 . . ? C6 C13 H13A 109.1 . . ? C6 C13 H13B 109.1 . . ? C6 C13 C14 112.3(4) . . ? H13A C13 H13B 107.9 . . ? C14 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? O3 C21 C1 110.6(3) . . ? O2 C21 O3 124.4(4) . . ? O2 C21 C1 124.9(4) . . ? C9 C10 H10 119.0 . . ? C9 C10 C11 122.0(4) . . ? C11 C10 H10 119.0 . . ? C13 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C15 C14 C13 113.6(4) . . ? C15 C14 H14A 108.8 . . ? C15 C14 H14B 108.8 . . ? C6 C5 H5A 108.7 . . ? C6 C5 H5B 108.7 . . ? C4 C5 C6 114.3(3) . . ? C4 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? O1 C23 N2 121.6(4) . . ? O1 C23 C24 118.6(4) . . ? N2 C23 C24 119.8(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C18 C17 C16 120.0(5) . . ? C24 C25 H25 120.1 . . ? C24 C25 C26 119.9(5) . . ? C26 C25 H25 120.1 . . ? N1 C8 C7 107.4(4) . . ? N1 C8 C9 130.3(4) . . ? C9 C8 C7 122.3(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.5 . . ? C3 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C3 C2 C1 112.4(3) . . ? H2A C2 H2B 107.9 . . ? C1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C25 C24 C23 122.0(4) . . ? C25 C24 C29 119.6(4) . . ? C29 C24 C23 118.0(4) . . ? N2 C1 C21 110.8(3) . . ? N2 C1 C2 110.5(4) . . ? N2 C1 H1A 106.8 . . ? C21 C1 C2 114.7(3) . . ? C21 C1 H1A 106.8 . . ? C2 C1 H1A 106.8 . . ? C25 C26 H26 120.3 . . ? C27 C26 C25 119.5(4) . . ? C27 C26 H26 120.3 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.2(5) . . ? C20 C19 H19 119.9 . . ? C26 C27 Br1 118.8(4) . . ? C26 C27 C28 121.5(5) . . ? C28 C27 Br1 119.6(4) . . ? C17 C18 H18 120.3 . . ? C19 C18 C17 119.4(5) . . ? C19 C18 H18 120.3 . . ? C16 C15 C14 120.7(4) . . ? C16 C15 C20 118.2(5) . . ? C20 C15 C14 121.1(5) . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C24 C29 H29 120.0 . . ? C28 C29 C24 120.0(4) . . ? C28 C29 H29 120.0 . . ? C27 C28 C29 119.5(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? O3 C22 H22A 109.5 . . ? O3 C22 H22B 109.5 . . ? O3 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C20 C15 121.3(6) . . ? C19 C20 H20 119.3 . . ? C15 C20 H20 119.3 . . ? 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 C27 1.896(5) . ? O1 C23 1.235(5) . ? C3 C4 1.375(6) . ? C3 C7 1.436(6) . ? C3 C2 1.504(6) . ? O3 C21 1.329(5) . ? O3 C22 1.439(6) . ? N1 H1 0.8600 . ? N1 C4 1.386(6) . ? N1 C8 1.372(5) . ? O2 C21 1.205(5) . ? N2 C6 1.473(5) . ? N2 C23 1.349(6) . ? N2 C1 1.469(6) . ? C6 H6 0.9800 . ? C6 C13 1.527(6) . ? C6 C5 1.549(5) . ? C4 C5 1.499(6) . ? C7 C12 1.400(6) . ? C7 C8 1.413(6) . ? C9 H9 0.9300 . ? C9 C10 1.386(6) . ? C9 C8 1.393(6) . ? C12 H12 0.9300 . ? C12 C11 1.390(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.536(6) . ? C21 C1 1.518(6) . ? C10 H10 0.9300 . ? C10 C11 1.396(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.497(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C23 C24 1.507(6) . ? C17 H17 0.9300 . ? C17 C16 1.393(7) . ? C17 C18 1.379(7) . ? C25 H25 0.9300 . ? C25 C24 1.390(6) . ? C25 C26 1.396(7) . ? C16 H16 0.9300 . ? C16 C15 1.380(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C1 1.538(6) . ? C24 C29 1.398(7) . ? C1 H1A 0.9800 . ? C26 H26 0.9300 . ? C26 C27 1.374(8) . ? C19 H19 0.9300 . ? C19 C18 1.379(9) . ? C19 C20 1.380(8) . ? C27 C28 1.375(7) . ? C18 H18 0.9300 . ? C15 C20 1.384(7) . ? C11 H11 0.9300 . ? C29 H29 0.9300 . ? C29 C28 1.388(7) . ? C28 H28 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C20 H20 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 C27 C28 C29 -174.6(3) . . . . ? O1 C23 C24 C25 113.2(5) . . . . ? O1 C23 C24 C29 -59.0(5) . . . . ? C3 C4 C5 C6 -56.1(7) . . . . ? C3 C7 C12 C11 -178.5(5) . . . . ? C3 C7 C8 N1 -1.8(5) . . . . ? C3 C7 C8 C9 178.0(4) . . . . ? C3 C2 C1 N2 48.7(5) . . . . ? C3 C2 C1 C21 174.8(4) . . . . ? O3 C21 C1 N2 149.0(4) . . . . ? O3 C21 C1 C2 23.0(5) . . . . ? N1 C4 C5 C6 126.8(4) . . . . ? O2 C21 C1 N2 -35.4(6) . . . . ? O2 C21 C1 C2 -161.4(4) . . . . ? N2 C6 C13 C14 -166.9(4) . . . . ? N2 C6 C5 C4 39.4(5) . . . . ? N2 C23 C24 C25 -67.0(5) . . . . ? N2 C23 C24 C29 120.8(4) . . . . ? C6 N2 C23 O1 175.1(4) . . . . ? C6 N2 C23 C24 -4.7(6) . . . . ? C6 N2 C1 C21 132.1(4) . . . . ? C6 N2 C1 C2 -99.6(4) . . . . ? C6 C13 C14 C15 173.9(4) . . . . ? C4 C3 C7 C12 179.3(5) . . . . ? C4 C3 C7 C8 1.2(5) . . . . ? C4 C3 C2 C1 8.5(7) . . . . ? C4 N1 C8 C7 1.8(5) . . . . ? C4 N1 C8 C9 -178.0(4) . . . . ? C7 C3 C4 N1 -0.2(5) . . . . ? C7 C3 C4 C5 -177.6(5) . . . . ? C7 C3 C2 C1 -171.7(4) . . . . ? C7 C12 C11 C10 1.0(7) . . . . ? C9 C10 C11 C12 -0.6(7) . . . . ? C12 C7 C8 N1 179.7(4) . . . . ? C12 C7 C8 C9 -0.5(6) . . . . ? C13 C6 C5 C4 163.1(5) . . . . ? C13 C14 C15 C16 74.9(6) . . . . ? C13 C14 C15 C20 -106.6(6) . . . . ? C10 C9 C8 N1 -179.4(4) . . . . ? C10 C9 C8 C7 0.9(6) . . . . ? C14 C15 C20 C19 -179.4(5) . . . . ? C5 C6 C13 C14 69.3(5) . . . . ? C23 N2 C6 C13 106.9(5) . . . . ? C23 N2 C6 C5 -128.9(4) . . . . ? C23 N2 C1 C21 -57.3(5) . . . . ? C23 N2 C1 C2 71.0(4) . . . . ? C23 C24 C29 C28 171.4(4) . . . . ? C17 C16 C15 C14 178.6(4) . . . . ? C17 C16 C15 C20 0.0(7) . . . . ? C25 C24 C29 C28 -1.1(6) . . . . ? C25 C26 C27 Br1 176.2(4) . . . . ? C25 C26 C27 C28 0.1(7) . . . . ? C8 N1 C4 C3 -1.0(5) . . . . ? C8 N1 C4 C5 176.7(4) . . . . ? C8 C7 C12 C11 -0.5(6) . . . . ? C8 C9 C10 C11 -0.3(7) . . . . ? C16 C17 C18 C19 0.3(8) . . . . ? C16 C15 C20 C19 -0.8(8) . . . . ? C2 C3 C4 N1 179.6(4) . . . . ? C2 C3 C4 C5 2.2(8) . . . . ? C2 C3 C7 C12 -0.5(8) . . . . ? C2 C3 C7 C8 -178.6(4) . . . . ? C24 C25 C26 C27 -2.2(7) . . . . ? C24 C29 C28 C27 -0.9(7) . . . . ? C1 N2 C6 C13 -83.1(4) . . . . ? C1 N2 C6 C5 41.1(5) . . . . ? C1 N2 C23 O1 5.1(6) . . . . ? C1 N2 C23 C24 -174.8(4) . . . . ? C26 C25 C24 C23 -169.5(4) . . . . ? C26 C25 C24 C29 2.6(7) . . . . ? C26 C27 C28 C29 1.4(7) . . . . ? C18 C17 C16 C15 0.3(7) . . . . ? C18 C19 C20 C15 1.4(10) . . . . ? C22 O3 C21 O2 -3.6(7) . . . . ? C22 O3 C21 C1 172.0(4) . . . . ? C20 C19 C18 C17 -1.1(9) . . . . ?