#------------------------------------------------------------------------------ #$Date: 2020-10-23 07:36:19 +0300 (Fri, 23 Oct 2020) $ #$Revision: 258573 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/22/2022265.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022265 loop_ _publ_author_name 'Okezue, Mercy' 'Smith, Daniel' 'Zeller, Matthias' 'Byrn, Stephen R.' 'Smith, Pamela' 'Bogandowich-Knipp, Susan' 'Purcell, Dale K.' 'Clase, Kari L.' _publ_section_title ; Crystal structures of salts of bedaquiline ; _journal_coeditor_code OV3143 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229620013455 _journal_volume 76 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_iupac 'C32 H31 Br N2 O2' _chemical_formula_moiety 'C32 H31 Br N2 O2' _chemical_formula_sum 'C32 H31 Br N2 O2' _chemical_formula_weight 555.50 _chemical_name_common ; Bedaquline ; _chemical_name_systematic ; 1-(6-Bromo-2-methoxyquinolin-3-yl)-4-(dimethylamino)- 2-(naphthalen-1-yl)-1-phenylbutan-2-ol ; _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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 11.1584(8) _cell_length_b 13.6425(14) _cell_length_c 36.061(4) _cell_measurement_reflns_used 9979 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.6578 _cell_measurement_theta_min 2.4258 _cell_volume 5489.5(9) _computing_cell_refinement ; SAINT (Bruker, 2019) ; _computing_data_collection ; APEX3 (Bruker, 2019) ; _computing_data_reduction ; SAINT (Bruker, 2019) ; _computing_molecular_graphics ; Mercury (Macrae et al., 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015) and shelXle (H\"ubschle et al., 2011) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 7.4074 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.910 _diffrn_measurement_device_type ; Bruker D8 Quest diffractometer with PhotonII charge-integrating pixel array detector (CPAD) ; _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'Triumph curved graphite crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_unetI/netI 0.0711 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 66520 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.160 _diffrn_reflns_theta_min 2.258 _diffrn_source 'fine focus sealed tube X-ray source' _diffrn_source_current '30 mA' _diffrn_source_voltage '50 kV' _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS2016; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.344 _exptl_crystal_description plate _exptl_crystal_F_000 2304 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.480 _refine_diff_density_min -0.584 _refine_ls_abs_structure_details ; Flack x determined using 4397 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.034(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 675 _refine_ls_number_reflns 17893 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0441 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+2.4789P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.1111 _reflns_number_gt 12296 _reflns_number_total 17893 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ov3143sup1.cif _cod_data_source_block 1 _cod_database_code 2022265 _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 0.740 _shelx_estimated_absorpt_t_max 0.927 _shelx_hkl_file ; 2 0 0 498.195 38.3958 2 -2 0 0 504.120 38.4869 2 -2 0 0 452.111 38.3777 2 -3 0 0 6.97158 1.34378 2 -3 0 0 7.81284 1.43901 2 3 0 0 10.7736 1.51143 2 4 0 0 3370.93 266.677 2 -5 0 0 6.70157 1.55117 2 5 0 0 2.49778 1.72195 2 -5 0 0 5.27549 1.39735 2 -6 0 0 1459.32 113.378 2 -6 0 0 1358.43 113.358 2 6 0 0 1479.89 113.454 2 7 0 0 23.9999 3.18528 2 -7 0 0 32.3972 3.06250 2 -7 0 0 30.7457 3.05219 2 8 0 0 568.541 45.2750 2 10 0 0 34.7043 4.44779 2 11 0 0 16.0052 3.38828 2 12 0 0 12.2937 3.55277 2 13 0 0 -0.0318 3.50295 2 14 0 0 79.8584 8.78505 2 15 0 0 3.13469 4.22718 2 16 0 0 -4.0993 4.06348 2 1 1 0 109.077 9.84397 2 1 -1 0 130.219 9.62787 2 -2 -1 0 139.123 11.4117 2 2 1 0 150.864 11.4456 2 2 -1 0 134.637 11.2534 2 3 1 0 979.268 77.6927 2 -3 -1 0 944.596 77.6704 2 -3 -1 0 978.647 77.6886 2 3 -1 0 1019.82 77.6218 2 -4 -1 0 79.6455 6.96816 2 4 -1 0 84.6984 6.77039 2 -4 -1 0 84.2556 7.07267 2 4 1 0 73.6191 7.10436 2 -5 -1 0 466.450 37.2366 2 5 1 0 472.448 37.2722 2 5 -1 0 470.983 37.1674 2 -5 -1 0 461.942 37.2067 2 6 -1 0 17.0646 2.41519 2 6 1 0 19.5875 2.74368 2 -6 -1 0 24.6950 2.63350 2 -6 -1 0 23.0803 2.52272 2 7 1 0 14.3554 2.62274 2 -7 -1 0 14.6797 2.34864 2 7 -1 0 14.4158 2.19416 2 -7 -1 0 14.7538 2.44465 2 -8 -1 0 375.170 30.6672 2 -8 -1 0 388.819 30.7106 2 8 1 0 390.893 30.8835 2 -9 -1 0 108.958 9.53500 2 9 1 0 122.759 10.2262 2 -9 -1 0 112.735 9.50702 2 10 -1 0 231.865 18.9664 2 11 -1 0 7.84677 2.99111 2 11 1 0 10.1175 3.44096 2 12 -1 0 26.1317 3.81771 2 12 1 0 20.8742 4.22290 2 13 -1 0 5.08094 3.26725 2 13 1 0 4.41178 3.97756 2 14 -1 0 5.27041 3.74082 2 14 1 0 -2.6486 4.12082 2 15 1 0 8.09564 4.76102 2 15 -1 0 9.85717 3.77985 2 16 -1 0 6.39039 3.98225 2 16 1 0 5.73363 5.19925 2 17 1 0 3.13503 4.53101 2 0 2 0 921.249 72.3233 2 0 -2 0 905.259 72.3150 2 -1 -2 0 610.167 49.5208 2 1 2 0 607.256 49.5261 2 -1 -2 0 682.526 49.5246 2 1 -2 0 605.319 49.4672 2 1 -2 0 636.791 49.4781 2 -1 2 0 604.857 49.4734 2 2 -2 0 176.665 12.9755 2 2 2 0 158.032 13.1525 2 2 -2 0 152.686 12.9332 2 -2 -2 0 158.001 13.1545 2 -3 -2 0 13.2157 2.22722 2 3 2 0 18.2204 2.36545 2 4 -2 0 1954.44 149.001 2 -4 -2 0 1813.55 149.090 2 -4 -2 0 1845.81 149.085 2 4 2 0 1918.42 149.115 2 5 2 0 3.81570 2.19452 2 -5 -2 0 1.63489 2.12224 2 5 -2 0 2.35638 1.42732 2 -5 -2 0 3.56685 2.00576 2 -6 -2 0 23.0492 2.82255 2 -6 -2 0 24.5179 2.98904 2 6 2 0 19.8121 3.01831 2 6 -2 0 23.0084 2.47067 2 -7 -2 0 500.987 39.3369 2 -7 -2 0 509.206 39.3862 2 7 -2 0 483.915 39.2936 2 7 2 0 480.333 39.4392 2 8 2 0 147.046 12.4369 2 -8 -2 0 145.884 12.0916 2 -8 -2 0 147.071 12.1896 2 8 -2 0 140.145 12.0658 2 -9 -2 0 483.113 39.2527 2 9 2 0 487.180 39.4656 2 9 -2 0 511.768 39.2241 2 -9 -2 0 486.095 39.2909 2 10 -2 0 43.4086 4.58586 2 10 2 0 36.8961 4.40250 2 -10 -2 0 26.1850 3.60326 2 -11 -2 0 163.106 12.8496 2 11 -2 0 162.056 13.1880 2 11 2 0 136.402 14.7584 2 -11 -2 0 152.354 12.8260 2 12 -2 0 69.2870 6.98318 2 12 2 0 62.7485 6.97868 2 13 -2 0 9.84863 3.12521 2 13 2 0 12.0297 4.23780 2 14 -2 0 62.6113 6.30804 2 14 2 0 44.4631 6.24095 2 15 2 0 7.04188 5.33016 2 15 -2 0 5.43899 3.20146 2 16 2 0 6.05462 5.63103 2 0 -3 0 3.38568 1.72255 2 0 -3 0 1.57432 1.71214 2 0 3 0 1.07865 1.71023 2 1 -3 0 1651.50 131.039 2 -1 -3 0 1637.11 131.071 2 1 3 0 1671.92 131.075 2 -1 -3 0 1658.00 131.068 2 1 -3 0 1658.46 131.033 2 2 -3 0 138.456 11.8175 2 2 3 0 137.825 12.3344 2 2 -3 0 143.447 11.8549 2 -2 -3 0 163.506 12.1043 2 -2 -3 0 147.688 12.0943 2 -2 3 0 142.833 11.8491 2 3 -3 0 83.0490 6.82876 2 3 3 0 83.3583 7.33618 2 3 -3 0 76.3376 6.77530 2 -3 -3 0 75.9828 7.24183 2 4 -3 0 6.92413 1.69395 2 -4 -3 0 6.04622 2.23233 2 4 -3 0 11.4089 1.61229 2 4 3 0 5.46194 2.30931 2 -5 -3 0 211.633 17.2019 2 5 -3 0 212.233 16.8862 2 -5 -3 0 206.462 17.2210 2 5 3 0 211.066 17.3069 2 -6 -3 0 190.413 16.2862 2 -6 -3 0 191.305 16.3206 2 6 3 0 192.692 16.4056 2 6 -3 0 215.048 15.9632 2 7 3 0 56.5883 6.03907 2 -7 -3 0 54.1128 5.66277 2 -7 -3 0 44.2397 5.74949 2 -8 -3 0 206.722 16.6781 2 8 -3 0 203.227 16.2888 2 -8 -3 0 199.582 16.6105 2 8 3 0 195.917 16.8072 2 -9 -3 0 6.53493 2.84408 2 9 -3 0 9.79391 2.06029 2 9 3 0 4.75611 3.22663 2 -9 -3 0 4.34304 2.69978 2 -10 -3 0 0.82557 2.78158 2 10 -3 0 6.11763 2.20783 2 -10 -3 0 1.26665 2.92297 2 10 3 0 5.56333 3.49485 2 11 3 0 44.6331 5.43791 2 -11 -3 0 38.0983 4.62965 2 -11 -3 0 41.6307 4.67795 2 11 -3 0 52.2635 5.18414 2 12 3 0 117.049 11.3495 2 12 -3 0 121.337 10.0382 2 -12 -3 0 107.150 10.0158 2 13 -3 0 28.3071 3.66073 2 13 3 0 24.1172 5.16188 2 14 3 0 35.8996 5.59677 2 14 -3 0 33.0903 3.92851 2 15 3 0 16.9002 5.22062 2 0 4 0 25.1045 2.83009 2 0 -4 0 21.7556 2.84789 2 0 -4 0 20.4839 2.83748 2 -1 -4 0 647.923 47.3449 2 1 4 0 605.535 47.3219 2 -1 4 0 567.691 47.2572 2 1 -4 0 564.363 47.2567 2 -1 -4 0 623.488 47.3542 2 1 -4 0 561.418 47.2748 2 -2 -4 0 408.451 32.6548 2 2 4 0 407.572 32.6505 2 2 -4 0 399.828 32.5374 2 2 -4 0 408.757 32.5146 2 -2 4 0 409.015 32.5111 2 -2 -4 0 415.070 32.6625 2 -3 -4 0 785.184 62.9153 2 3 -4 0 746.564 62.7696 2 3 4 0 806.239 62.9365 2 -3 4 0 829.655 62.7683 2 -3 -4 0 813.099 62.9394 2 3 -4 0 770.691 62.7944 2 -4 -4 0 99.7715 8.52582 2 4 4 0 98.1311 8.59797 2 4 -4 0 94.8945 7.98052 2 4 -4 0 85.1217 7.99016 2 5 -4 0 150.808 11.6946 2 5 -4 0 139.571 11.7118 2 -5 -4 0 136.186 12.1247 2 5 4 0 142.848 12.2960 2 6 -4 0 413.250 32.4042 2 6 -4 0 408.765 32.3987 2 6 4 0 418.782 32.7395 2 -6 -4 0 386.643 32.6793 2 7 -4 0 775.322 59.2938 2 -7 -4 0 755.580 59.5103 2 7 -4 0 733.355 59.3265 2 -7 -4 0 765.986 59.5529 2 7 4 0 706.311 59.5544 2 -8 -4 0 24.7052 3.79992 2 8 4 0 30.3295 4.09950 2 8 -4 0 31.2405 3.65637 2 8 -4 0 31.8686 3.79291 2 -8 -4 0 30.8261 4.01749 2 -9 -4 0 35.9461 4.39223 2 -9 -4 0 30.9065 4.29258 2 9 -4 0 43.1798 4.21237 2 9 4 0 30.5823 4.67881 2 9 -4 0 37.3957 4.30968 2 -10 -4 0 41.1295 5.01278 2 10 -4 0 46.1702 4.91024 2 10 -4 0 43.3607 4.85340 2 10 4 0 48.4678 5.48570 2 -11 -4 0 280.783 23.8997 2 11 4 0 302.018 24.3572 2 11 -4 0 293.996 23.4769 2 -12 -4 0 48.5026 5.46055 2 12 -4 0 57.0446 5.39503 2 12 -4 0 50.2383 5.32720 2 12 4 0 49.4038 6.30898 2 13 -4 0 24.6278 3.18991 2 13 -4 0 27.5601 3.06482 2 14 4 0 6.18327 5.15887 2 15 4 0 5.10089 5.34295 2 0 5 0 2.11376 2.29272 2 0 -5 0 6.46515 2.32654 2 1 5 0 28.0125 3.42250 2 -1 -5 0 29.6688 3.55392 2 1 -5 0 30.7508 3.29680 2 -1 -5 0 26.8944 3.42079 2 1 -5 0 30.1352 3.38993 2 -2 -5 0 43.3647 5.38140 2 2 -5 0 40.5288 4.71382 2 2 -5 0 38.8463 4.07630 2 -2 -5 0 41.1837 5.17543 2 -2 5 0 43.5208 4.69955 2 2 5 0 40.7087 4.31006 2 -3 -5 0 562.431 44.9012 2 3 5 0 559.093 44.9226 2 3 -5 0 565.303 44.7838 2 3 -5 0 559.744 44.7478 2 -3 5 0 569.937 44.7427 2 -3 -5 0 559.478 44.9375 2 -4 -5 0 47.7169 6.15060 2 4 5 0 45.9172 6.16952 2 4 -5 0 60.1369 5.37656 2 -4 -5 0 65.5648 6.24055 2 4 -5 0 47.5875 5.43173 2 5 -5 0 226.548 19.1713 2 -5 -5 0 245.284 19.5493 2 5 -5 0 243.051 19.1960 2 6 5 0 12.4561 3.25495 2 -6 -5 0 16.5596 3.16708 2 6 -5 0 18.4450 2.43818 2 6 -5 0 17.6722 2.44782 2 7 5 0 193.215 16.1054 2 7 -5 0 188.543 15.3462 2 -7 -5 0 185.204 15.8987 2 -8 -5 0 28.3435 4.43746 2 8 5 0 27.2560 4.46618 2 -8 -5 0 27.5034 4.27411 2 8 -5 0 38.0359 4.18972 2 8 -5 0 43.4373 4.10052 2 -9 -5 0 27.9488 3.90176 2 9 -5 0 16.8476 2.73179 2 9 -5 0 22.3646 2.90071 2 -9 -5 0 25.5898 4.10767 2 9 5 0 28.2187 4.28214 2 -10 -5 0 24.0343 4.57440 2 10 5 0 28.4358 4.91488 2 10 -5 0 35.6242 4.15854 2 -10 -5 0 32.4395 4.57831 2 10 -5 0 35.0630 4.12175 2 11 -5 0 32.3643 3.27181 2 11 -5 0 35.6621 4.10483 2 11 5 0 20.8167 5.12926 2 -11 -5 0 24.9512 4.56858 2 12 5 0 14.1898 4.73515 2 -12 -5 0 1.10734 3.69459 2 12 -5 0 4.36164 1.98558 2 13 5 0 75.6315 9.57763 2 -13 -5 0 75.4475 8.33391 2 14 5 0 -0.2929 5.10889 2 15 5 0 1.55380 6.17201 2 0 6 0 129.288 10.7490 2 0 -6 0 129.708 10.8249 2 0 -6 0 111.061 10.7007 2 -1 6 0 263.910 21.9568 2 -1 -6 0 273.803 22.0705 2 1 6 0 277.235 22.0788 2 1 -6 0 288.066 22.0161 2 1 -6 0 246.078 22.2636 2 -1 -6 0 275.870 22.1184 2 2 -6 0 1024.10 79.9575 2 2 -6 0 991.204 79.9909 2 -2 -6 0 1003.33 80.0426 2 -2 6 0 998.929 79.9475 2 -2 -6 0 1007.19 80.0673 2 2 6 0 1020.45 80.0556 2 -3 6 0 161.406 12.9910 2 -3 -6 0 158.072 13.3313 2 3 -6 0 152.487 13.0889 2 -3 -6 0 147.281 13.4166 2 3 -6 0 154.385 13.0290 2 3 6 0 163.212 13.4903 2 -4 -6 0 70.0662 7.20106 2 4 -6 0 65.5718 6.66375 2 4 6 0 73.9201 7.50292 2 -4 -6 0 68.4286 7.43382 2 4 -6 0 63.8942 6.62775 2 -4 6 0 71.9799 6.35407 2 5 6 0 447.115 37.5951 2 -5 -6 0 479.804 37.6099 2 5 -6 0 477.262 37.3343 2 5 -6 0 463.967 37.3312 2 -5 -6 0 471.137 37.6248 2 -6 -6 0 45.9835 5.42733 2 6 6 0 46.3085 5.50344 2 6 -6 0 58.5274 5.49868 2 6 -6 0 61.4983 5.52933 2 7 -6 0 73.8400 6.54344 2 -7 -6 0 84.2984 7.64183 2 -7 -6 0 53.8220 7.04575 2 7 6 0 64.0305 7.85845 2 8 6 0 45.9732 6.22646 2 -8 -6 0 59.9571 7.31627 2 8 -6 0 59.9743 5.92029 2 8 -6 0 66.6118 5.83011 2 -8 -6 0 58.8601 6.57927 2 9 -6 0 392.216 32.8701 2 9 6 0 403.449 33.6227 2 9 -6 0 408.529 32.8743 2 -9 -6 0 423.365 33.4159 2 -9 -6 0 433.496 33.4560 2 10 -6 0 99.4347 8.79575 2 10 6 0 97.8410 11.0528 2 -10 -6 0 106.961 10.2995 2 -10 -6 0 98.9216 10.3583 2 10 -6 0 102.367 8.79270 2 11 -6 0 5.61115 1.96673 2 -11 -6 0 4.27483 3.93351 2 11 -6 0 2.43727 2.05080 2 11 6 0 3.77110 4.56556 2 12 6 0 48.4213 6.69721 2 -13 -6 0 136.120 12.9906 2 13 6 0 139.180 14.1433 2 -14 -6 0 4.50939 3.60916 2 0 7 0 3.92219 2.65999 2 0 -7 0 2.68965 2.70041 2 -1 -7 0 -2.4104 2.72849 2 -1 7 0 4.91264 2.54593 2 -1 -7 0 -2.1453 2.92205 2 1 7 0 3.77614 2.83031 2 1 -7 0 4.03735 2.60933 2 2 -7 0 149.243 12.4786 2 -2 -7 0 139.609 12.9233 2 2 -7 0 141.513 12.5700 2 -2 7 0 156.366 12.4168 2 2 7 0 150.926 12.7848 2 -2 -7 0 136.609 12.6640 2 -3 -7 0 53.2095 7.18340 2 3 -7 0 67.9988 6.62483 2 3 7 0 59.2301 7.30566 2 -3 7 0 62.6030 6.34373 2 -3 -7 0 57.9825 6.98554 2 3 -7 0 69.0856 6.46669 2 4 -7 0 762.736 63.1703 2 4 7 0 796.962 63.4079 2 -4 -7 0 786.735 63.3740 2 4 -7 0 795.412 63.2030 2 -4 7 0 805.267 63.1371 2 -4 -7 0 822.968 63.4308 2 5 -7 0 259.021 21.0105 2 -5 -7 0 273.942 21.5374 2 -5 -7 0 248.369 22.0095 2 5 7 0 261.022 21.4640 2 5 -7 0 251.481 21.0173 2 -6 -7 0 351.301 29.1766 2 6 -7 0 338.567 28.8483 2 6 7 0 368.271 29.3790 2 -6 -7 0 366.039 29.3384 2 6 -7 0 373.301 28.8619 2 -7 -7 0 -1.8248 3.35510 2 7 -7 0 3.78487 2.90034 2 7 -7 0 4.78437 2.43399 2 7 7 0 2.00815 3.62395 2 8 7 0 101.443 11.7926 2 8 -7 0 97.7108 9.31389 2 -8 -7 0 110.959 10.5686 2 8 -7 0 110.133 9.23802 2 -8 -7 0 101.108 10.4032 2 9 -7 0 3.99995 2.51846 2 9 -7 0 11.2332 2.59301 2 9 7 0 5.55106 4.33447 2 -9 -7 0 8.56431 4.31656 2 -10 -7 0 12.0501 4.67911 2 10 -7 0 11.4320 2.55415 2 10 7 0 6.60543 4.57683 2 -10 -7 0 13.8288 4.75827 2 10 -7 0 11.5620 2.62091 2 11 7 0 34.5671 6.36196 2 11 -7 0 48.8864 4.59157 2 -11 -7 0 31.3053 5.50596 2 11 -7 0 37.2703 4.64351 2 12 7 0 76.4633 8.57599 2 -12 -7 0 70.7932 7.75849 2 -13 -7 0 4.30855 4.32338 2 13 7 0 8.84027 5.76031 2 14 7 0 -1.6446 5.92386 2 0 -8 0 195.275 17.0510 2 0 -8 0 210.411 17.2868 2 0 8 0 208.522 17.0941 2 1 -8 0 465.752 38.1678 2 -1 -8 0 473.980 38.1732 2 -1 8 0 488.611 38.1028 2 1 -8 0 465.554 38.1127 2 -1 -8 0 473.074 38.2251 2 1 8 0 482.999 38.1709 2 -2 -8 0 -2.2336 3.01717 2 2 -8 0 6.43325 2.90684 2 2 8 0 0.43334 3.01665 2 -2 -8 0 2.44823 3.36413 2 2 -8 0 3.97054 2.65336 2 3 -8 0 320.721 26.7443 2 -3 8 0 336.314 26.6473 2 3 -8 0 317.177 26.6496 2 3 8 0 346.196 26.9894 2 -3 -8 0 339.173 27.0753 2 -3 -8 0 321.784 26.8976 2 4 -8 0 40.0817 4.33684 2 -4 -8 0 33.1731 4.94695 2 -4 8 0 41.4267 4.15388 2 -4 -8 0 34.2532 4.70218 2 4 8 0 36.5684 4.77065 2 4 -8 0 37.5742 4.17818 2 -5 -8 0 454.121 37.0310 2 5 -8 0 454.536 36.6560 2 5 -8 0 449.294 36.6529 2 5 8 0 484.886 37.0906 2 -5 -8 0 445.636 36.9690 2 6 -8 0 24.4066 3.31122 2 6 8 0 18.0185 4.26146 2 -6 -8 0 18.6618 4.47252 2 6 -8 0 18.2217 3.31966 2 -6 -8 0 21.0700 4.08898 2 -7 -8 0 8.37652 4.11541 2 -7 -8 0 12.2081 3.94885 2 7 -8 0 7.08984 2.83164 2 7 8 0 14.7442 4.24179 2 7 -8 0 -1.7612 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5 -3 28 135.338 13.8331 2 -5 3 28 128.205 11.6425 2 -5 3 28 124.756 11.1758 2 5 3 28 119.831 13.0025 2 -5 3 -28 111.990 12.9893 2 5 -3 -28 126.724 12.0042 2 -5 -3 28 114.723 12.1142 2 6 3 -28 31.8082 5.91724 2 -6 3 28 39.4029 4.77578 2 -6 -3 -28 40.2810 6.45022 2 6 -3 28 38.8853 6.49234 2 -6 3 28 41.6863 4.42797 2 -6 -3 28 36.0711 5.63123 2 -6 -3 28 45.9643 5.87009 2 6 -3 -28 42.5828 6.17355 2 6 3 28 36.5558 6.61968 2 -6 3 -28 31.5873 6.16444 2 -7 -3 -28 14.3125 6.28807 2 7 -3 28 30.4112 6.14582 2 -7 3 28 26.4797 3.65576 2 -7 3 28 26.0853 3.46549 2 7 3 -28 28.7157 5.66407 2 -7 -3 28 32.3393 5.29669 2 7 -3 -28 39.7121 4.96791 2 -7 -3 28 39.7732 5.25612 2 7 3 28 33.4467 6.59907 2 -8 -3 -28 59.7380 7.66342 2 8 3 -28 55.0802 6.86349 2 8 -3 28 59.9569 7.51563 2 -8 -3 28 56.9588 6.31156 2 8 -3 -28 56.7337 6.19642 2 8 3 28 46.4446 7.71770 2 -8 3 -28 45.8856 6.92594 2 9 3 -28 35.2809 5.85367 2 9 -3 28 42.2938 6.58546 2 9 -3 -28 41.9519 5.39534 2 -9 3 -28 37.7239 6.19174 2 9 3 28 34.4896 7.02618 2 -9 -3 28 35.0130 5.17545 2 10 3 -28 39.1431 5.87818 2 10 -3 28 32.8648 6.59448 2 -10 -3 28 33.5126 4.45371 2 10 -3 -28 38.8673 5.05862 2 -10 3 -28 28.0045 5.73325 2 10 3 28 34.6827 7.01072 2 -11 -3 -28 12.4859 6.01424 2 11 -3 28 5.73922 5.66691 2 11 3 28 13.2653 6.32658 2 11 -3 -28 20.4996 4.12509 2 -11 3 -28 11.2503 4.78222 2 -12 -3 -28 37.2809 7.12739 2 12 3 -28 50.0520 6.79423 2 12 -3 28 56.7186 7.79260 2 12 -3 -28 52.6649 5.51806 2 12 3 28 46.5111 8.37783 2 -12 3 -28 46.4678 6.19032 2 0 -4 -28 45.7999 6.19175 2 0 -4 28 36.2066 7.65553 2 0 -4 28 40.8570 6.22893 2 0 4 28 45.4648 5.85591 2 0 4 -28 48.8075 6.50691 2 1 -4 28 141.833 14.7952 2 -1 4 28 145.107 14.2526 2 -1 -4 -28 160.632 14.8213 2 1 -4 28 132.566 14.9617 2 1 4 -28 162.087 14.7900 2 1 4 28 154.002 14.4637 2 -1 4 -28 163.664 14.8730 2 -1 -4 28 180.920 14.7406 2 -1 -4 28 161.239 15.0384 2 1 -4 -28 161.514 14.6501 2 2 -4 28 55.6686 6.88764 2 2 4 -28 62.7050 6.90699 2 2 -4 28 47.9681 6.89907 2 -2 4 28 56.1794 6.00933 2 -2 -4 -28 46.6654 6.66012 2 2 4 28 54.0210 6.73108 2 2 -4 -28 61.0503 6.47747 2 -2 -4 28 45.7598 6.49449 2 -2 -4 28 34.5260 6.57100 2 3 -4 28 127.057 14.4818 2 -3 4 28 142.418 13.0721 2 -3 -4 -28 137.828 14.2077 2 3 -4 28 140.699 14.2721 2 3 4 -28 145.911 13.9702 2 3 4 28 162.949 14.3165 2 3 -4 -28 154.414 13.7786 2 -3 -4 28 145.696 14.1495 2 -3 4 -28 156.637 14.1591 2 -3 -4 28 144.299 13.9286 2 4 -4 28 298.160 27.8578 2 -4 -4 -28 317.056 28.0574 2 -4 4 28 325.128 27.0310 2 -4 4 28 341.610 27.3899 2 4 4 -28 319.083 27.8167 2 4 -4 28 319.184 28.2230 2 4 -4 -28 353.596 27.4886 2 -4 4 -28 334.617 27.9328 2 4 4 28 351.605 28.4066 2 -4 -4 28 351.863 27.6707 2 5 -4 28 31.9366 6.24150 2 5 -4 28 40.1944 6.62276 2 5 4 -28 34.0229 5.99167 2 -5 4 28 30.8240 4.86810 2 -5 -4 -28 36.2551 6.36668 2 -5 4 -28 41.8312 6.37237 2 -5 -4 28 40.6405 5.67884 2 5 -4 -28 35.8298 5.39162 2 5 4 28 40.5377 6.59956 2 -5 -4 28 27.7999 5.64688 2 6 -4 28 7.98202 5.41719 2 6 -4 28 15.3188 5.85351 2 6 4 -28 8.63744 5.13415 2 -6 4 28 11.8247 3.01473 2 -6 -4 -28 11.7625 5.82087 2 -6 -4 28 15.6333 4.79317 2 -6 4 -28 13.7055 4.88970 2 6 -4 -28 9.48180 4.18461 2 -6 -4 28 10.2270 4.84899 2 6 4 28 18.9047 5.85452 2 -7 4 28 10.5579 2.45395 2 7 -4 28 3.88343 5.27566 2 7 4 -28 12.5393 5.00316 2 -7 4 28 7.71274 2.22591 2 -7 -4 -28 13.4601 5.76446 2 -7 -4 28 6.36184 4.81024 2 7 4 28 10.6484 5.74486 2 7 -4 -28 9.15857 4.18083 2 8 4 -28 43.2010 7.09868 2 8 -4 28 63.5518 8.18223 2 8 -4 28 45.1137 7.46687 2 -8 -4 -28 52.7046 7.69357 2 8 4 -28 43.9673 7.39593 2 -8 4 -28 70.8497 8.78176 2 -8 -4 28 59.9017 6.59157 2 8 4 28 63.0482 7.97900 2 8 -4 -28 79.3626 7.75565 2 9 4 -28 33.1254 6.50458 2 9 4 -28 36.1706 6.02065 2 9 -4 28 39.8577 7.24629 2 -9 -4 -28 35.2055 6.68874 2 9 -4 -28 31.2406 4.96116 2 9 4 28 35.5503 7.05859 2 -9 4 -28 30.4462 5.68710 2 10 4 -28 -0.4639 5.51381 2 10 -4 28 2.45597 6.45825 2 10 4 -28 3.18069 5.03872 2 10 -4 28 9.76655 5.59882 2 10 4 28 -3.4600 6.33074 2 10 -4 -28 9.48225 3.87039 2 -10 4 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-51 6.26300 9.09124 2 1 1 51 -4.4614 8.93131 2 2 1 -51 4.00054 9.18460 2 2 -1 51 1.09404 9.85925 2 -2 -1 -51 -1.2408 9.18004 2 2 -1 -51 -3.7953 9.16245 2 2 1 51 8.38276 10.3604 2 -2 1 -51 11.0293 10.8300 2 -3 -1 -51 -7.9717 10.0848 2 3 1 -51 -3.8746 8.71304 2 3 -1 51 9.49409 10.3141 2 -3 1 -51 -2.5154 9.83934 2 3 -1 -51 5.84947 9.58254 2 3 1 51 3.36769 11.5040 2 -4 -1 -51 0.06954 9.29448 2 4 -1 51 -7.4711 10.5634 2 4 1 51 -6.1739 10.8139 2 -4 1 -51 1.52151 10.0202 2 -5 -1 -51 11.9324 11.1806 2 5 -1 51 1.71632 11.7503 2 5 1 51 15.0651 12.1745 2 6 -1 51 6.48675 12.1748 2 6 1 51 2.62112 12.4213 2 0 2 -51 6.65935 9.16721 2 0 -2 -51 3.46677 9.40223 2 0 -2 51 -4.9142 9.39300 2 1 2 -51 5.12771 9.31228 2 -1 -2 -51 9.55072 10.0501 2 1 -2 51 -7.9949 9.94370 2 -1 2 -51 8.37540 9.61633 2 1 -2 -51 13.9182 9.41671 2 -2 -2 -51 0.38191 9.73856 2 2 -2 51 -0.0726 9.58681 2 2 2 -51 -3.3721 8.98084 2 -2 2 -51 -4.4797 9.85552 2 2 -2 -51 -6.7371 9.09224 2 2 2 51 19.1395 10.8205 2 -3 -2 -51 4.32083 10.9410 2 3 2 -51 9.55196 9.02901 2 -3 2 -51 9.90839 9.52267 2 3 2 51 9.66231 11.0898 2 4 -2 51 5.57685 10.2694 2 -4 -2 -51 10.3506 10.4415 2 -4 2 -51 6.23597 10.0739 2 -5 -2 -51 5.87114 10.6858 2 5 -2 51 6.89926 10.0513 2 5 2 51 3.55796 11.5521 2 6 -2 51 0.51373 10.8011 2 6 2 51 -6.5280 11.4594 2 0 3 -51 16.7522 9.56975 2 0 -3 51 -4.8441 10.1579 2 -1 -3 -51 28.4631 10.5311 2 1 -3 51 10.6030 9.85389 2 1 3 -51 29.9531 9.79539 2 -1 3 -51 26.8025 10.5875 2 1 -3 -51 25.6103 10.6650 2 2 3 -51 -4.4618 9.37814 2 2 -3 51 31.1370 11.1831 2 -2 -3 -51 -1.5633 10.6369 2 -2 3 -51 5.71448 9.18077 2 2 -3 -51 4.74653 9.25101 2 3 -3 51 12.5220 9.86422 2 3 3 -51 16.8110 9.44487 2 -3 -3 -51 6.76820 10.3906 2 -3 3 -51 6.18857 9.87417 2 4 -3 51 3.22026 9.85607 2 -4 -3 -51 8.28186 11.4398 2 -4 3 -51 4.85001 9.43300 2 5 -3 51 3.67297 10.9024 2 -5 -3 -51 0.72289 10.2111 2 0 4 -51 7.61214 9.66533 2 0 -4 -51 16.9712 10.3947 2 1 4 -51 6.05387 9.50417 2 1 -4 51 10.1626 10.9612 2 -1 4 -51 -1.1614 9.89118 2 1 -4 -51 6.63230 9.36482 2 -2 -4 -51 -1.1768 10.3742 2 2 4 -51 8.17007 10.0295 2 -2 4 -51 8.85016 10.3606 2 3 -4 51 -1.3291 10.3210 2 3 4 -51 1.48021 9.06404 2 -3 -4 -51 9.36098 10.5462 2 -3 4 -51 6.81790 9.88857 2 4 -4 51 -15.335 10.9489 2 -4 -4 -51 4.97992 10.7689 2 5 -4 51 -2.2847 10.8710 2 -5 -4 -51 11.6358 11.2757 2 0 -5 -51 10.5502 9.77475 2 0 5 -51 2.60880 9.97954 2 -1 -5 -51 -4.8307 9.91652 2 1 -5 51 -0.1903 10.9643 2 1 5 -51 -6.0831 9.38904 2 -1 5 -51 6.16899 9.43857 2 1 -5 -51 12.1117 11.0119 2 2 -5 51 34.4713 11.3447 2 2 5 -51 32.8569 9.99789 2 -2 5 -51 26.1575 10.6636 2 3 -5 51 8.81668 10.5594 2 -3 -5 -51 1.89225 10.7456 2 3 5 -51 5.85750 9.56404 2 -3 5 -51 15.7348 9.64996 2 -4 -5 -51 -9.4020 11.1901 2 4 -5 51 -13.702 10.3693 2 0 6 -51 0.56216 10.0099 2 0 -6 -51 9.11998 11.7565 2 1 6 -51 8.87764 10.1055 2 -1 -6 -51 4.21333 10.2736 2 -1 6 -51 0.53530 9.78530 2 2 -6 51 7.76527 10.2811 2 -2 -6 -51 9.02334 9.69405 2 2 6 -51 -3.8644 9.37803 2 -2 6 -51 -3.8919 9.82567 2 3 -6 51 2.11181 10.4477 2 3 6 -51 -11.642 9.06685 2 -4 -6 -51 1.86430 11.5499 2 4 -6 51 -5.0059 11.4365 2 0 7 -51 -1.4047 10.0517 2 -1 7 -51 7.29885 10.3885 2 2 7 -51 9.82938 9.67835 2 -2 -7 -51 -2.9237 11.1795 2 -3 -7 -51 3.30572 11.4670 2 3 -7 51 10.6653 12.7190 2 0 8 -51 9.12051 10.3866 2 0 0 -52 5.06570 9.77157 2 1 0 -52 1.11970 9.82056 2 -1 0 -52 -5.0297 9.83677 2 2 0 -52 56.2680 10.9454 2 -2 0 -52 59.9910 12.0147 2 -3 0 -52 4.62111 10.2623 2 3 0 52 13.9531 11.1046 2 4 0 52 8.21507 11.7957 2 -4 0 -52 -7.2382 9.50780 2 5 0 52 0.34956 11.7912 2 0 1 -52 -4.0593 9.45644 2 1 1 -52 -2.2115 11.3273 2 -1 -1 -52 17.7325 10.3997 2 -1 1 -52 0.87463 10.6113 2 1 -1 -52 1.43103 9.49070 2 2 1 -52 13.6865 9.61725 2 -2 -1 -52 -0.1156 10.3615 2 2 -1 52 22.1435 11.5005 2 -2 1 -52 10.6540 9.67935 2 2 -1 -52 1.57310 9.45914 2 -3 -1 -52 -4.0505 11.0903 2 -3 1 -52 6.60570 10.3727 2 4 -1 52 -1.9536 10.1363 2 -4 -1 -52 2.87483 10.5552 2 4 1 52 6.06944 12.4445 2 -4 1 -52 6.74756 10.3675 2 5 -1 52 8.42732 11.4286 2 0 -2 -52 -2.9806 10.8856 2 0 2 -52 6.70408 9.75916 2 -1 -2 -52 -8.6042 10.5941 2 1 -2 -52 -5.5146 10.1679 2 -1 2 -52 -7.9944 9.66055 2 -2 -2 -52 -3.0018 9.30554 2 2 2 -52 1.66323 9.27643 2 2 -2 52 -10.852 10.2501 2 -2 2 -52 4.21068 9.39370 2 2 -2 -52 1.57486 10.5863 2 3 -2 52 6.39961 10.5350 2 3 2 -52 -6.8738 10.6141 2 -3 -2 -52 -13.564 10.8965 2 -3 2 -52 -2.9020 9.68433 2 4 -2 52 1.42361 10.1225 2 -4 -2 -52 -3.0021 9.43514 2 -4 2 -52 4.15817 10.9797 2 5 -2 52 -5.7314 11.1845 2 0 3 -52 4.68457 9.64786 2 0 -3 -52 0.22793 9.92182 2 -1 3 -52 8.76412 9.63502 2 1 -3 -52 3.00819 10.1651 2 2 -3 52 4.91549 10.6375 2 -2 -3 -52 4.50530 9.85969 2 2 3 -52 6.14855 9.65229 2 -2 3 -52 5.00195 9.41116 2 3 -3 52 -9.7163 10.8454 2 -3 -3 -52 5.17932 10.6849 2 3 3 -52 -5.0743 10.4279 2 -3 3 -52 -2.9388 10.3188 2 4 -3 52 -2.1053 10.9848 2 -4 -3 -52 11.4662 9.75450 2 5 -3 52 5.22680 11.5849 2 0 4 -52 7.44304 10.1118 2 0 -4 -52 17.7229 10.1586 2 -1 -4 -52 -2.6610 10.3736 2 -1 4 -52 -1.4465 10.0723 2 2 4 -52 8.34245 9.48449 2 -2 4 -52 7.98769 10.2648 2 3 -4 52 0.97835 10.5526 2 -3 -4 -52 10.2641 11.6447 2 -3 4 -52 -0.9366 10.0145 2 4 -4 52 -1.1301 11.4336 2 -4 -4 -52 14.6956 11.6796 2 0 5 -52 3.85276 9.96732 2 0 -5 -52 3.12941 10.4026 2 -1 -5 -52 1.57551 10.1608 2 -1 5 -52 -14.462 9.85963 2 2 5 -52 -6.5118 9.49195 2 -2 -5 -52 7.47314 11.2847 2 -2 5 -52 -17.611 9.70079 2 3 -5 52 3.91469 12.6032 2 -4 -5 -52 -5.6663 10.9620 2 4 -5 52 6.39848 10.8863 2 0 6 -52 23.0577 10.7654 2 -1 -6 -52 6.58345 11.5210 2 1 6 -52 11.0595 10.9048 2 -1 6 -52 5.36496 10.2564 2 2 6 -52 -6.3830 10.0148 2 -2 -6 -52 1.89278 9.48034 2 -3 -6 -52 18.6282 11.8107 2 0 7 -52 11.0775 10.5930 2 1 7 -52 -10.755 10.0500 2 1 0 -53 8.04661 10.0221 2 -1 0 -53 8.22482 10.4648 2 2 0 -53 -2.0891 11.1598 2 -2 0 -53 4.97967 10.5747 2 -3 0 -53 -13.496 11.1238 2 -4 0 -53 -1.1779 11.7502 2 0 -1 -53 -8.1453 9.95423 2 1 1 -53 3.09781 9.78546 2 -1 1 -53 11.6614 10.2672 2 1 -1 -53 0.80741 9.54202 2 2 1 -53 8.12823 9.60927 2 -2 -1 -53 7.96508 9.90700 2 -2 1 -53 5.29251 10.5026 2 -3 -1 -53 1.77956 10.7352 2 -3 1 -53 2.41283 10.5628 2 -4 -1 -53 -6.4632 9.95404 2 0 -2 -53 1.23282 10.2375 2 1 2 -53 3.46941 9.61822 2 -1 2 -53 7.32155 10.2841 2 1 -2 -53 -10.155 9.77024 2 -2 -2 -53 10.3339 10.5968 2 2 2 -53 10.5085 9.52680 2 -2 2 -53 -4.3892 10.2323 2 -3 -2 -53 3.53914 10.7137 2 -3 2 -53 0.20967 10.7772 2 -4 -2 -53 13.3023 12.0625 2 0 -3 -53 7.02703 10.4747 2 0 3 -53 -3.6643 12.1005 2 1 3 -53 4.27994 9.72920 2 -1 -3 -53 0.81806 11.2380 2 -1 3 -53 -4.1623 9.89151 2 2 3 -53 9.43635 9.84524 2 -2 3 -53 5.17804 10.1733 2 -3 -3 -53 21.4766 11.4863 2 -3 3 -53 5.15473 10.9918 2 -4 -3 -53 5.53000 10.6636 2 0 -4 -53 0.21108 11.0951 2 1 4 -53 15.7164 10.1159 2 -1 -4 -53 5.24796 10.8339 2 -1 4 -53 4.97072 10.1391 2 2 4 -53 -6.0597 9.45001 2 -2 -4 -53 14.8451 11.3661 2 -2 4 -53 3.53957 10.3908 2 1 5 -53 -2.8652 10.1009 2 -1 5 -53 0.12875 10.4145 2 2 5 -53 8.52439 10.4157 2 -2 -5 -53 9.11400 11.6567 2 1 6 -53 -0.2206 10.5182 2 -1 6 -53 -5.3869 10.4998 2 0 0 -54 17.9398 10.5627 2 1 0 -54 -15.962 9.71782 2 -2 0 -54 37.3661 11.0591 2 -3 0 -54 -4.0534 10.6879 2 0 1 -54 -4.0377 10.7201 2 0 -1 -54 -5.3125 10.6437 2 -1 -1 -54 0.76227 10.6784 2 1 1 -54 -1.8361 9.61759 2 -2 1 -54 3.44402 10.6122 2 -3 -1 -54 -0.1897 11.8365 2 -3 1 -54 0.59858 11.5804 2 0 2 -54 8.70005 10.2341 2 0 -2 -54 -2.8096 10.2302 2 -1 -2 -54 6.53271 10.6561 2 1 2 -54 18.2056 11.1201 2 -1 2 -54 13.9235 10.7472 2 -2 2 -54 -2.1485 10.4280 2 -3 -2 -54 -7.2018 10.8007 2 0 3 -54 -1.1471 10.6486 2 1 3 -54 -9.1132 9.96989 2 -1 -3 -54 -2.3711 10.3792 2 -1 3 -54 12.1216 10.6496 2 -2 -3 -54 -17.580 11.1002 2 -2 3 -54 -0.1291 10.3376 2 0 4 -54 -0.2254 10.4156 2 1 4 -54 16.6697 10.3372 2 -1 4 -54 -10.944 10.3108 2 -2 -4 -54 6.83153 11.0643 2 0 0 -55 -3.8653 10.3199 2 -1 0 -55 1.88269 10.7776 2 0 1 -55 -11.303 9.37839 2 -1 -1 -55 0.15516 11.4360 2 -1 1 -55 9.73961 10.6098 2 -2 -1 -55 -3.7803 9.87158 2 0 2 -55 -1.5041 10.2431 2 -1 -2 -55 13.6907 11.5633 2 -1 2 -55 0.85861 11.4786 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6031 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71076 11.155 13.643 36.055 89.993 90.004 90.000 ) ; _shelx_hkl_checksum 78595 _shelx_res_file ; TITL MaleicACN_0m_a.res in P2(1)2(1)2(1) 1.res created by SHELXL-2018/3 at 13:34:10 on 31-Aug-2020 REM Old TITL MaleicACN_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.159, Rweak 0.056, Alpha 0.026, Orientation as input REM Flack x = 0.048 ( 0.013 ) from Parsons' quotients REM Formula found by SHELXT: C64 N3 O5 Br2 CELL 0.71073 11.1584 13.6425 36.0610 90.000 90.000 90.000 ZERR 8.000 0.0008 0.0014 0.0038 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H Br N O UNIT 256 248 8 16 16 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.150 SIZE 0.21 0.13 0.05 OMIT 1 0 3 OMIT 9 4 0 OMIT -5 1 10 OMIT 0 0 4 L.S. 14 BOND $H ACTA CONF FMAP 2 PLAN 20 HTAB HTAB O1 N1 HTAB C1 O2 HTAB O3 N3 HTAB C33 O4 MPLA C1 C23 > C32 O2 N2 Br1 MPLA C1 C17 > C22 MPLA C2 C7 > C16 MPLA C1 C23 > C32 O2 N2 Br1 MPLA C33 C55 > C63 O4 N4 Br2 MPLA C33 C49 > C54 MPLA C34 C39 > C48 MPLA C33 C55 > C63 O4 N4 Br2 WGHT 0.029800 2.478900 FVAR 0.30214 BR1 3 -0.224175 0.598926 0.934034 11.00000 0.02814 0.06708 = 0.04775 -0.00632 0.00642 -0.00323 O1 5 0.323794 0.600840 0.796187 11.00000 0.02922 0.03517 = 0.02560 -0.00228 -0.00350 -0.00118 AFIX 147 H1O 2 0.296203 0.640769 0.780645 11.00000 -1.50000 AFIX 0 O2 5 0.482783 0.725088 0.908558 11.00000 0.03019 0.03675 = 0.02637 -0.00941 -0.00096 -0.00498 N1 4 0.300838 0.768114 0.757007 11.00000 0.03750 0.04851 = 0.02617 0.00377 -0.00038 0.00416 N2 4 0.296775 0.723271 0.935790 11.00000 0.03147 0.03288 = 0.02230 -0.00264 0.00207 -0.00069 C1 1 0.433652 0.590807 0.853258 11.00000 0.02315 0.02469 = 0.02687 -0.00128 0.00175 -0.00088 AFIX 13 H1 2 0.511656 0.613215 0.863960 11.00000 -1.20000 AFIX 0 C2 1 0.421810 0.644368 0.815223 11.00000 0.02639 0.02599 = 0.02580 -0.00147 0.00119 -0.00166 C3 1 0.391146 0.754131 0.819955 11.00000 0.02818 0.02959 = 0.02848 -0.00257 0.00010 0.00272 AFIX 23 H3A 2 0.311884 0.760086 0.832083 11.00000 -1.20000 H3B 2 0.451320 0.784829 0.836451 11.00000 -1.20000 AFIX 0 C4 1 0.388501 0.809578 0.783089 11.00000 0.03210 0.03267 = 0.03436 0.00461 0.00262 0.00131 AFIX 23 H4A 2 0.368347 0.879127 0.787832 11.00000 -1.20000 H4B 2 0.469185 0.807406 0.771700 11.00000 -1.20000 AFIX 0 C5 1 0.180667 0.805756 0.764419 11.00000 0.03661 0.07796 = 0.05023 0.00454 -0.00857 0.01020 AFIX 137 H5A 2 0.181362 0.877472 0.762872 11.00000 -1.50000 H5B 2 0.155422 0.785688 0.789317 11.00000 -1.50000 H5C 2 0.124585 0.779366 0.746042 11.00000 -1.50000 AFIX 0 C6 1 0.335163 0.789067 0.718260 11.00000 0.07151 0.06196 = 0.02861 0.01040 0.00165 0.00471 AFIX 137 H6A 2 0.274637 0.761942 0.701453 11.00000 -1.50000 H6B 2 0.413095 0.759038 0.712972 11.00000 -1.50000 H6C 2 0.340535 0.860126 0.714641 11.00000 -1.50000 AFIX 0 C7 1 0.537736 0.634948 0.791835 11.00000 0.03070 0.02710 = 0.02981 0.00225 0.00460 0.00352 C8 1 0.530348 0.587893 0.758142 11.00000 0.04268 0.03515 = 0.02951 -0.00111 0.00785 0.00491 AFIX 43 H8 2 0.459085 0.553241 0.752149 11.00000 -1.20000 AFIX 0 C9 1 0.625442 0.589382 0.732085 11.00000 0.05146 0.04218 = 0.03732 0.00352 0.01714 0.01245 AFIX 43 H9 2 0.617529 0.555399 0.709222 11.00000 -1.20000 AFIX 0 C10 1 0.726949 0.638835 0.739656 11.00000 0.04623 0.05249 = 0.04509 0.01097 0.02316 0.01342 AFIX 43 H10 2 0.788893 0.641601 0.721614 11.00000 -1.20000 AFIX 0 C11 1 0.742614 0.686681 0.774071 11.00000 0.03266 0.04046 = 0.05609 0.01451 0.01462 0.00499 C12 1 0.849840 0.736336 0.781987 11.00000 0.03297 0.05939 = 0.08586 0.01997 0.01990 -0.00053 AFIX 43 H12 2 0.910315 0.740322 0.763505 11.00000 -1.20000 AFIX 0 C13 1 0.868886 0.779005 0.815731 11.00000 0.03256 0.05898 = 0.09566 0.00516 0.00673 -0.00959 AFIX 43 H13 2 0.942439 0.811591 0.820635 11.00000 -1.20000 AFIX 0 C14 1 0.781076 0.774797 0.842791 11.00000 0.03571 0.05215 = 0.07094 0.00690 -0.00385 -0.01492 AFIX 43 H14 2 0.795439 0.803479 0.866381 11.00000 -1.20000 AFIX 0 C15 1 0.673571 0.729661 0.835902 11.00000 0.03292 0.03299 = 0.04732 0.00340 -0.00036 -0.00175 AFIX 43 H15 2 0.613991 0.729114 0.854720 11.00000 -1.20000 AFIX 0 C16 1 0.648852 0.683696 0.801397 11.00000 0.03187 0.02904 = 0.04044 0.00758 0.00435 0.00309 C17 1 0.440617 0.479142 0.852271 11.00000 0.02702 0.02637 = 0.02790 -0.00352 0.00453 0.00218 C18 1 0.524225 0.434179 0.875468 11.00000 0.03724 0.03207 = 0.03909 0.00153 0.00054 0.00336 AFIX 43 H18 2 0.578525 0.473635 0.889212 11.00000 -1.20000 AFIX 0 C19 1 0.529628 0.332938 0.878860 11.00000 0.04098 0.03626 = 0.05937 0.01062 0.00060 0.00735 AFIX 43 H19 2 0.586943 0.304062 0.894989 11.00000 -1.20000 AFIX 0 C20 1 0.452329 0.273795 0.858971 11.00000 0.04257 0.02758 = 0.07039 0.00291 0.01429 0.00731 AFIX 43 H20 2 0.455743 0.204480 0.861264 11.00000 -1.20000 AFIX 0 C21 1 0.370555 0.317374 0.835842 11.00000 0.04282 0.02949 = 0.06372 -0.00937 0.00331 -0.00016 AFIX 43 H21 2 0.317076 0.277449 0.821984 11.00000 -1.20000 AFIX 0 C22 1 0.364268 0.418312 0.832256 11.00000 0.03824 0.02728 = 0.04661 -0.00659 -0.00227 -0.00032 AFIX 43 H22 2 0.307030 0.446401 0.815903 11.00000 -1.20000 AFIX 0 C23 1 0.337474 0.623294 0.880944 11.00000 0.03106 0.02413 = 0.02130 -0.00103 0.00187 0.00041 C24 1 0.221498 0.592497 0.880150 11.00000 0.02973 0.02509 = 0.02507 -0.00239 0.00138 -0.00028 AFIX 43 H24 2 0.196272 0.548059 0.861430 11.00000 -1.20000 AFIX 0 C25 1 0.137481 0.626044 0.907029 11.00000 0.02638 0.02562 = 0.02646 0.00245 0.00012 0.00010 C26 1 0.015133 0.598375 0.906910 11.00000 0.02843 0.03241 = 0.03010 -0.00064 0.00301 0.00254 AFIX 43 H26 2 -0.014665 0.554893 0.888515 11.00000 -1.20000 AFIX 0 C27 1 -0.059437 0.634909 0.933530 11.00000 0.02318 0.04240 = 0.03419 0.00218 0.00190 0.00255 C28 1 -0.019004 0.699701 0.961251 11.00000 0.03172 0.04918 = 0.02993 -0.00462 0.00575 0.00328 AFIX 43 H28 2 -0.073061 0.724205 0.979370 11.00000 -1.20000 AFIX 0 C29 1 0.099026 0.726962 0.961792 11.00000 0.03174 0.04382 = 0.02698 -0.00694 0.00282 0.00243 AFIX 43 H29 2 0.126805 0.770477 0.980477 11.00000 -1.20000 AFIX 0 C30 1 0.180374 0.691036 0.934797 11.00000 0.03163 0.02999 = 0.02199 0.00219 0.00003 0.00367 C31 1 0.368847 0.691105 0.909784 11.00000 0.02552 0.02819 = 0.02415 0.00071 -0.00346 -0.00048 C32 1 0.518095 0.794467 0.936488 11.00000 0.03209 0.04701 = 0.03492 -0.01301 -0.00539 -0.00776 AFIX 137 H32A 2 0.601622 0.813868 0.932406 11.00000 -1.50000 H32B 2 0.510293 0.764395 0.961050 11.00000 -1.50000 H32C 2 0.466450 0.852445 0.935054 11.00000 -1.50000 AFIX 0 BR2 3 1.503188 0.528374 0.980769 11.00000 0.04355 0.05500 = 0.04227 -0.00133 -0.00983 -0.00769 O3 5 1.113748 0.174374 0.870330 11.00000 0.03009 0.03053 = 0.04151 -0.00051 0.01286 0.00246 AFIX 147 H3O 2 1.149698 0.120544 0.872362 11.00000 -1.50000 AFIX 0 O4 5 0.831842 0.304602 0.958903 11.00000 0.03507 0.04990 = 0.04155 -0.00796 0.01754 -0.00552 N3 4 1.159442 -0.008123 0.894389 11.00000 0.03944 0.03417 = 0.03874 -0.00590 0.00391 0.00728 N4 4 0.986367 0.392509 0.984799 11.00000 0.04916 0.03498 = 0.02528 0.00054 0.00907 0.00360 C33 1 0.944435 0.267214 0.891833 11.00000 0.02927 0.03181 = 0.02744 -0.00121 0.00441 0.00020 AFIX 13 H33 2 0.859615 0.258280 0.900123 11.00000 -1.20000 AFIX 0 C34 1 0.991915 0.163230 0.882375 11.00000 0.02950 0.02799 = 0.02977 -0.00031 0.00780 -0.00168 C35 1 0.994824 0.096934 0.917119 11.00000 0.03372 0.03096 = 0.03162 0.00284 0.00633 0.00216 AFIX 23 H35A 2 1.050174 0.125785 0.935591 11.00000 -1.20000 H35B 2 0.913825 0.095086 0.928300 11.00000 -1.20000 AFIX 0 C36 1 1.034743 -0.007427 0.908531 11.00000 0.03640 0.03337 = 0.03976 0.00145 0.00390 0.00016 AFIX 23 H36A 2 1.029756 -0.047775 0.931298 11.00000 -1.20000 H36B 2 0.980637 -0.036456 0.889749 11.00000 -1.20000 AFIX 0 C37 1 1.245639 -0.008150 0.924833 11.00000 0.04013 0.05802 = 0.05850 -0.00882 -0.00114 0.00829 AFIX 137 H37A 2 1.327104 -0.004144 0.914792 11.00000 -1.50000 H37B 2 1.237028 -0.068711 0.939203 11.00000 -1.50000 H37C 2 1.230662 0.048388 0.940944 11.00000 -1.50000 AFIX 0 C38 1 1.182088 -0.091333 0.869708 11.00000 0.06648 0.03737 = 0.04924 -0.01142 0.01087 0.01083 AFIX 137 H38A 2 1.126162 -0.089017 0.848772 11.00000 -1.50000 H38B 2 1.170719 -0.152677 0.883403 11.00000 -1.50000 H38C 2 1.264538 -0.087986 0.860431 11.00000 -1.50000 AFIX 0 C39 1 0.916652 0.117282 0.850701 11.00000 0.04335 0.02804 = 0.02786 0.00059 0.00872 -0.00080 C40 1 0.970780 0.103967 0.817125 11.00000 0.05353 0.05474 = 0.03565 -0.01037 0.01604 -0.01261 AFIX 43 H40 2 1.050579 0.126813 0.814025 11.00000 -1.20000 AFIX 0 C41 1 0.914133 0.058020 0.786853 11.00000 0.07483 0.06550 = 0.03129 -0.01419 0.01271 -0.01660 AFIX 43 H41 2 0.955036 0.052016 0.763861 11.00000 -1.20000 AFIX 0 C42 1 0.802073 0.022585 0.790452 11.00000 0.06876 0.04676 = 0.03106 -0.00969 0.00191 -0.00949 AFIX 43 H42 2 0.764721 -0.009785 0.770191 11.00000 -1.20000 AFIX 0 C43 1 0.740106 0.033554 0.824346 11.00000 0.04718 0.02891 = 0.03477 -0.00089 -0.00219 -0.00350 C44 1 0.622852 -0.004952 0.828138 11.00000 0.04772 0.03952 = 0.04418 -0.00017 -0.01083 -0.00529 AFIX 43 H44 2 0.587964 -0.039705 0.808023 11.00000 -1.20000 AFIX 0 C45 1 0.559201 0.006824 0.859997 11.00000 0.04519 0.04190 = 0.05344 0.00949 -0.00923 -0.00927 AFIX 43 H45 2 0.481437 -0.020876 0.862275 11.00000 -1.20000 AFIX 0 C46 1 0.609229 0.060282 0.889560 11.00000 0.03627 0.04155 = 0.03898 0.01064 0.00239 -0.00116 AFIX 43 H46 2 0.563583 0.070801 0.911439 11.00000 -1.20000 AFIX 0 C47 1 0.722389 0.097092 0.887134 11.00000 0.03790 0.03022 = 0.03020 0.00244 0.00226 -0.00015 AFIX 43 H47 2 0.754336 0.132226 0.907619 11.00000 -1.20000 AFIX 0 C48 1 0.794403 0.084595 0.854854 11.00000 0.04062 0.02457 = 0.03051 0.00268 0.00208 -0.00022 C49 1 0.940212 0.339940 0.859523 11.00000 0.02823 0.02763 = 0.02901 -0.00284 0.00096 -0.00149 C50 1 0.841920 0.400703 0.857050 11.00000 0.03395 0.03652 = 0.03939 -0.00219 0.00038 0.00356 AFIX 43 H50 2 0.777022 0.391304 0.873727 11.00000 -1.20000 AFIX 0 C51 1 0.834791 0.475355 0.830897 11.00000 0.04550 0.04136 = 0.04444 0.00243 -0.00494 0.00932 AFIX 43 H51 2 0.766337 0.516697 0.830043 11.00000 -1.20000 AFIX 0 C52 1 0.927434 0.489009 0.806264 11.00000 0.05069 0.04311 = 0.03888 0.01103 -0.00765 0.00235 AFIX 43 H52 2 0.922986 0.539544 0.788192 11.00000 -1.20000 AFIX 0 C53 1 1.027234 0.428779 0.807916 11.00000 0.04059 0.05800 = 0.03904 0.01679 0.00319 0.00129 AFIX 43 H53 2 1.091198 0.438060 0.790888 11.00000 -1.20000 AFIX 0 C54 1 1.034343 0.354679 0.834403 11.00000 0.02889 0.04670 = 0.03722 0.00849 0.00269 0.00623 AFIX 43 H54 2 1.103315 0.313947 0.835444 11.00000 -1.20000 AFIX 0 C55 1 1.009759 0.316056 0.924099 11.00000 0.03082 0.02479 = 0.02830 0.00139 0.00444 0.00432 C56 1 1.126576 0.344827 0.922806 11.00000 0.03745 0.02821 = 0.02362 -0.00075 0.00620 -0.00062 AFIX 43 H56 2 1.173876 0.328393 0.901803 11.00000 -1.20000 AFIX 0 C57 1 1.179173 0.399186 0.952417 11.00000 0.03530 0.02860 = 0.02343 0.00403 0.00317 0.00263 C58 1 1.298870 0.430032 0.952372 11.00000 0.03273 0.03432 = 0.02750 0.00230 0.00112 0.00139 AFIX 43 H58 2 1.350752 0.411765 0.932661 11.00000 -1.20000 AFIX 0 C59 1 1.340564 0.486587 0.980869 11.00000 0.03985 0.03519 = 0.03086 0.00487 -0.00676 -0.00055 C60 1 1.265894 0.515981 1.010259 11.00000 0.05479 0.04205 = 0.02605 -0.00273 -0.00494 0.00291 AFIX 43 H60 2 1.296029 0.556768 1.029467 11.00000 -1.20000 AFIX 0 C61 1 1.149056 0.484985 1.010812 11.00000 0.06146 0.03918 = 0.02342 -0.00420 0.00395 0.00430 AFIX 43 H61 2 1.098304 0.504605 1.030619 11.00000 -1.20000 AFIX 0 C62 1 1.102889 0.424562 0.982541 11.00000 0.04220 0.02890 = 0.02496 0.00217 0.00351 0.00407 C63 1 0.945365 0.340133 0.957309 11.00000 0.03359 0.02994 = 0.03116 0.00217 0.00800 0.00201 C64 1 0.762822 0.327578 0.991617 11.00000 0.04717 0.07000 = 0.04865 -0.00435 0.03032 -0.00250 AFIX 137 H64A 2 0.755306 0.398868 0.994016 11.00000 -1.50000 H64B 2 0.803387 0.301156 1.013550 11.00000 -1.50000 H64C 2 0.682908 0.298312 0.989498 11.00000 -1.50000 AFIX 0 HKLF 4 REM MaleicACN_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.1111, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0441 for 12296 Fo > 4sig(Fo) and 0.0836 for all 17893 data REM 675 parameters refined using 0 restraints END WGHT 0.0299 2.4766 REM Instructions for potential hydrogen bonds HTAB O1 N1 HTAB C1 O2 HTAB O3 N3 HTAB C33 O4 REM Highest difference peak 0.480, deepest hole -0.584, 1-sigma level 0.065 Q1 1 -0.2246 0.6860 0.9325 11.00000 0.05 0.48 Q2 1 1.5207 0.4573 0.9784 11.00000 0.05 0.45 Q3 1 1.4981 0.6176 0.9812 11.00000 0.05 0.45 Q4 1 -0.2271 0.4934 0.9371 11.00000 0.05 0.39 Q5 1 -0.1860 0.5259 0.9316 11.00000 0.05 0.33 Q6 1 1.5518 0.4012 0.9835 11.00000 0.05 0.33 Q7 1 1.4483 0.4584 0.9848 11.00000 0.05 0.29 Q8 1 1.3377 0.5780 0.9818 11.00000 0.05 0.27 Q9 1 1.4396 0.4034 0.9812 11.00000 0.05 0.26 Q10 1 1.5802 0.5992 0.9839 11.00000 0.05 0.25 Q11 1 0.9650 0.5972 0.8060 11.00000 0.05 0.24 Q12 1 0.8944 -0.0581 0.7938 11.00000 0.05 0.23 Q13 1 -0.2824 0.5210 0.9322 11.00000 0.05 0.23 Q14 1 0.0446 0.5339 0.8842 11.00000 0.05 0.23 Q15 1 0.2358 0.7344 0.9305 11.00000 0.05 0.23 Q16 1 0.4711 0.5421 0.8588 11.00000 0.05 0.23 Q17 1 0.7125 0.5204 0.8107 11.00000 0.05 0.22 Q18 1 -0.1416 0.7003 0.9395 11.00000 0.05 0.22 Q19 1 0.1616 0.8007 0.9563 11.00000 0.05 0.22 Q20 1 0.1974 0.4841 0.8815 11.00000 0.05 0.22 ; _shelx_res_checksum 50877 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 -0.22418(4) 0.59893(4) 0.93403(2) 0.04766(11) Uani d 1 . . O O1 0.3238(2) 0.60084(19) 0.79619(6) 0.0300(5) Uani d 1 . . H H1O 0.296203 0.640769 0.780645 0.045 Uiso calc 1 . . O O2 0.4828(2) 0.72509(17) 0.90856(6) 0.0311(5) Uani d 1 . . N N1 0.3008(3) 0.7681(3) 0.75701(9) 0.0374(7) Uani d 1 . . N N2 0.2968(2) 0.7233(2) 0.93579(8) 0.0289(6) Uani d 1 . . C C1 0.4337(3) 0.5908(2) 0.85326(9) 0.0249(6) Uani d 1 . . H H1 0.511656 0.613215 0.863960 0.030 Uiso calc 1 . . C C2 0.4218(3) 0.6444(2) 0.81522(9) 0.0261(6) Uani d 1 . . C C3 0.3911(3) 0.7541(2) 0.81996(10) 0.0287(7) Uani d 1 . . H H3A 0.311884 0.760086 0.832083 0.034 Uiso calc 1 . . H H3B 0.451320 0.784829 0.836451 0.034 Uiso calc 1 . . C C4 0.3885(3) 0.8096(3) 0.78309(10) 0.0330(7) Uani d 1 . . H H4A 0.368347 0.879127 0.787832 0.040 Uiso calc 1 . . H H4B 0.469185 0.807406 0.771700 0.040 Uiso calc 1 . . C C5 0.1807(4) 0.8058(4) 0.76442(14) 0.0549(12) Uani d 1 . . H H5A 0.181362 0.877472 0.762872 0.082 Uiso calc 1 . . H H5B 0.155422 0.785688 0.789317 0.082 Uiso calc 1 . . H H5C 0.124585 0.779366 0.746042 0.082 Uiso calc 1 . . C C6 0.3352(5) 0.7891(4) 0.71826(12) 0.0540(12) Uani d 1 . . H H6A 0.274637 0.761942 0.701453 0.081 Uiso calc 1 . . H H6B 0.413095 0.759038 0.712972 0.081 Uiso calc 1 . . H H6C 0.340535 0.860126 0.714641 0.081 Uiso calc 1 . . C C7 0.5377(3) 0.6349(2) 0.79184(10) 0.0292(7) Uani d 1 . . C C8 0.5303(3) 0.5879(3) 0.75814(10) 0.0358(8) Uani d 1 . . H H8 0.459085 0.553241 0.752149 0.043 Uiso calc 1 . . C C9 0.6254(4) 0.5894(3) 0.73209(11) 0.0437(9) Uani d 1 . . H H9 0.617529 0.555399 0.709222 0.052 Uiso calc 1 . . C C10 0.7269(4) 0.6388(3) 0.73966(12) 0.0479(10) Uani d 1 . . H H10 0.788893 0.641601 0.721614 0.058 Uiso calc 1 . . C C11 0.7426(3) 0.6867(3) 0.77407(13) 0.0431(10) Uani d 1 . . C C12 0.8498(4) 0.7363(4) 0.78199(17) 0.0594(14) Uani d 1 . . H H12 0.910315 0.740322 0.763505 0.071 Uiso calc 1 . . C C13 0.8689(4) 0.7790(4) 0.81573(18) 0.0624(14) Uani d 1 . . H H13 0.942439 0.811591 0.820635 0.075 Uiso calc 1 . . C C14 0.7811(4) 0.7748(3) 0.84279(15) 0.0529(11) Uani d 1 . . H H14 0.795439 0.803479 0.866381 0.064 Uiso calc 1 . . C C15 0.6736(4) 0.7297(3) 0.83590(12) 0.0377(8) Uani d 1 . . H H15 0.613991 0.729114 0.854720 0.045 Uiso calc 1 . . C C16 0.6489(3) 0.6837(3) 0.80140(11) 0.0338(8) Uani d 1 . . C C17 0.4406(3) 0.4791(2) 0.85227(9) 0.0271(6) Uani d 1 . . C C18 0.5242(3) 0.4342(3) 0.87547(11) 0.0361(8) Uani d 1 . . H H18 0.578525 0.473635 0.889212 0.043 Uiso calc 1 . . C C19 0.5296(4) 0.3329(3) 0.87886(13) 0.0455(10) Uani d 1 . . H H19 0.586943 0.304062 0.894989 0.055 Uiso calc 1 . . C C20 0.4523(4) 0.2738(3) 0.85897(14) 0.0468(10) Uani d 1 . . H H20 0.455743 0.204480 0.861264 0.056 Uiso calc 1 . . C C21 0.3706(4) 0.3174(3) 0.83584(13) 0.0453(10) Uani d 1 . . H H21 0.317076 0.277449 0.821984 0.054 Uiso calc 1 . . C C22 0.3643(4) 0.4183(3) 0.83226(12) 0.0374(8) Uani d 1 . . H H22 0.307030 0.446401 0.815903 0.045 Uiso calc 1 . . C C23 0.3375(3) 0.6233(2) 0.88094(9) 0.0255(6) Uani d 1 . . C C24 0.2215(3) 0.5925(2) 0.88015(9) 0.0266(6) Uani d 1 . . H H24 0.196272 0.548059 0.861430 0.032 Uiso calc 1 . . C C25 0.1375(3) 0.6260(2) 0.90703(9) 0.0262(6) Uani d 1 . . C C26 0.0151(3) 0.5984(3) 0.90691(9) 0.0303(6) Uani d 1 . . H H26 -0.014665 0.554893 0.888515 0.036 Uiso calc 1 . . C C27 -0.0594(3) 0.6349(3) 0.93353(11) 0.0333(7) Uani d 1 . . C C28 -0.0190(3) 0.6997(3) 0.96125(10) 0.0369(8) Uani d 1 . . H H28 -0.073061 0.724205 0.979370 0.044 Uiso calc 1 . . C C29 0.0990(3) 0.7270(3) 0.96179(10) 0.0342(8) Uani d 1 . . H H29 0.126805 0.770477 0.980477 0.041 Uiso calc 1 . . C C30 0.1804(3) 0.6910(2) 0.93480(9) 0.0279(6) Uani d 1 . . C C31 0.3688(3) 0.6911(2) 0.90978(9) 0.0260(6) Uani d 1 . . C C32 0.5181(3) 0.7945(3) 0.93649(11) 0.0380(8) Uani d 1 . . H H32A 0.601622 0.813868 0.932406 0.057 Uiso calc 1 . . H H32B 0.510293 0.764395 0.961050 0.057 Uiso calc 1 . . H H32C 0.466450 0.852445 0.935054 0.057 Uiso calc 1 . . Br Br2 1.50319(4) 0.52837(3) 0.98077(2) 0.04694(11) Uani d 1 . . O O3 1.1137(2) 0.17437(18) 0.87033(7) 0.0340(5) Uani d 1 . . H H3O 1.149698 0.120544 0.872362 0.051 Uiso calc 1 . . O O4 0.8318(2) 0.3046(2) 0.95890(8) 0.0422(6) Uani d 1 . . N N3 1.1594(3) -0.0081(2) 0.89439(9) 0.0374(7) Uani d 1 . . N N4 0.9864(3) 0.3925(2) 0.98480(8) 0.0365(7) Uani d 1 . . C C33 0.9444(3) 0.2672(2) 0.89183(9) 0.0295(7) Uani d 1 . . H H33 0.859615 0.258280 0.900123 0.035 Uiso calc 1 . . C C34 0.9919(3) 0.1632(2) 0.88238(9) 0.0291(6) Uani d 1 . . C C35 0.9948(3) 0.0969(2) 0.91712(9) 0.0321(7) Uani d 1 . . H H35A 1.050174 0.125785 0.935591 0.039 Uiso calc 1 . . H H35B 0.913825 0.095086 0.928300 0.039 Uiso calc 1 . . C C36 1.0347(3) -0.0074(3) 0.90853(11) 0.0365(8) Uani d 1 . . H H36A 1.029756 -0.047775 0.931298 0.044 Uiso calc 1 . . H H36B 0.980637 -0.036456 0.889749 0.044 Uiso calc 1 . . C C37 1.2456(4) -0.0081(4) 0.92483(14) 0.0522(11) Uani d 1 . . H H37A 1.327104 -0.004144 0.914792 0.078 Uiso calc 1 . . H H37B 1.237028 -0.068711 0.939203 0.078 Uiso calc 1 . . H H37C 1.230662 0.048388 0.940944 0.078 Uiso calc 1 . . C C38 1.1821(4) -0.0913(3) 0.86971(13) 0.0510(11) Uani d 1 . . H H38A 1.126162 -0.089017 0.848772 0.077 Uiso calc 1 . . H H38B 1.170719 -0.152677 0.883403 0.077 Uiso calc 1 . . H H38C 1.264538 -0.087986 0.860431 0.077 Uiso calc 1 . . C C39 0.9167(3) 0.1173(2) 0.85070(10) 0.0331(8) Uani d 1 . . C C40 0.9708(4) 0.1040(3) 0.81713(11) 0.0480(10) Uani d 1 . . H H40 1.050579 0.126813 0.814025 0.058 Uiso calc 1 . . C C41 0.9141(5) 0.0580(4) 0.78685(12) 0.0572(13) Uani d 1 . . H H41 0.955036 0.052016 0.763861 0.069 Uiso calc 1 . . C C42 0.8021(4) 0.0226(3) 0.79045(11) 0.0489(11) Uani d 1 . . H H42 0.764721 -0.009785 0.770191 0.059 Uiso calc 1 . . C C43 0.7401(4) 0.0336(3) 0.82435(10) 0.0370(8) Uani d 1 . . C C44 0.6229(4) -0.0050(3) 0.82814(12) 0.0438(9) Uani d 1 . . H H44 0.587964 -0.039705 0.808023 0.053 Uiso calc 1 . . C C45 0.5592(4) 0.0068(3) 0.86000(13) 0.0468(10) Uani d 1 . . H H45 0.481437 -0.020876 0.862275 0.056 Uiso calc 1 . . C C46 0.6092(4) 0.0603(3) 0.88956(11) 0.0389(8) Uani d 1 . . H H46 0.563583 0.070801 0.911439 0.047 Uiso calc 1 . . C C47 0.7224(3) 0.0971(3) 0.88713(9) 0.0328(7) Uani d 1 . . H H47 0.754336 0.132226 0.907619 0.039 Uiso calc 1 . . C C48 0.7944(3) 0.0846(2) 0.85485(10) 0.0319(7) Uani d 1 . . C C49 0.9402(3) 0.3399(2) 0.85952(10) 0.0283(7) Uani d 1 . . C C50 0.8419(3) 0.4007(3) 0.85705(11) 0.0366(8) Uani d 1 . . H H50 0.777022 0.391304 0.873727 0.044 Uiso calc 1 . . C C51 0.8348(4) 0.4754(3) 0.83090(12) 0.0438(9) Uani d 1 . . H H51 0.766337 0.516697 0.830043 0.053 Uiso calc 1 . . C C52 0.9274(4) 0.4890(3) 0.80626(12) 0.0442(9) Uani d 1 . . H H52 0.922986 0.539544 0.788192 0.053 Uiso calc 1 . . C C53 1.0272(4) 0.4288(3) 0.80792(11) 0.0459(10) Uani d 1 . . H H53 1.091198 0.438060 0.790888 0.055 Uiso calc 1 . . C C54 1.0343(3) 0.3547(3) 0.83440(11) 0.0376(8) Uani d 1 . . H H54 1.103315 0.313947 0.835444 0.045 Uiso calc 1 . . C C55 1.0098(3) 0.3161(2) 0.92410(9) 0.0280(6) Uani d 1 . . C C56 1.1266(3) 0.3448(2) 0.92281(9) 0.0298(7) Uani d 1 . . H H56 1.173876 0.328393 0.901803 0.036 Uiso calc 1 . . C C57 1.1792(3) 0.3992(3) 0.95242(9) 0.0291(7) Uani d 1 . . C C58 1.2989(3) 0.4300(3) 0.95237(10) 0.0315(7) Uani d 1 . . H H58 1.350752 0.411765 0.932661 0.038 Uiso calc 1 . . C C59 1.3406(3) 0.4866(3) 0.98087(11) 0.0353(7) Uani d 1 . . C C60 1.2659(4) 0.5160(3) 1.01026(10) 0.0410(9) Uani d 1 . . H H60 1.296029 0.556768 1.029467 0.049 Uiso calc 1 . . C C61 1.1491(4) 0.4850(3) 1.01081(10) 0.0414(9) Uani d 1 . . H H61 1.098304 0.504605 1.030619 0.050 Uiso calc 1 . . C C62 1.1029(3) 0.4246(2) 0.98254(10) 0.0320(7) Uani d 1 . . C C63 0.9454(3) 0.3401(3) 0.95731(10) 0.0316(7) Uani d 1 . . C C64 0.7628(4) 0.3276(4) 0.99162(13) 0.0553(12) Uani d 1 . . H H64A 0.755306 0.398868 0.994016 0.083 Uiso calc 1 . . H H64B 0.803387 0.301156 1.013550 0.083 Uiso calc 1 . . H H64C 0.682908 0.298312 0.989498 0.083 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.02814(17) 0.0671(3) 0.0478(2) -0.00323(18) 0.00642(17) -0.0063(2) O1 0.0292(11) 0.0352(12) 0.0256(12) -0.0012(10) -0.0035(9) -0.0023(10) O2 0.0302(13) 0.0367(12) 0.0264(11) -0.0050(10) -0.0010(10) -0.0094(10) N1 0.0375(18) 0.0485(19) 0.0262(15) 0.0042(14) -0.0004(12) 0.0038(14) N2 0.0315(15) 0.0329(14) 0.0223(13) -0.0007(11) 0.0021(11) -0.0026(12) C1 0.0232(14) 0.0247(15) 0.0269(15) -0.0009(12) 0.0017(11) -0.0013(13) C2 0.0264(15) 0.0260(16) 0.0258(16) -0.0017(12) 0.0012(12) -0.0015(13) C3 0.0282(16) 0.0296(17) 0.0285(17) 0.0027(13) 0.0001(13) -0.0026(13) C4 0.0321(18) 0.0327(18) 0.0344(19) 0.0013(14) 0.0026(14) 0.0046(15) C5 0.037(2) 0.078(3) 0.050(3) 0.010(2) -0.0086(19) 0.005(2) C6 0.072(3) 0.062(3) 0.029(2) 0.005(2) 0.002(2) 0.010(2) C7 0.0307(17) 0.0271(16) 0.0298(17) 0.0035(12) 0.0046(13) 0.0022(13) C8 0.043(2) 0.0351(19) 0.0295(17) 0.0049(15) 0.0079(14) -0.0011(15) C9 0.051(2) 0.042(2) 0.037(2) 0.0125(19) 0.0171(17) 0.0035(18) C10 0.046(2) 0.052(2) 0.045(2) 0.013(2) 0.023(2) 0.0110(19) C11 0.033(2) 0.040(2) 0.056(3) 0.0050(15) 0.0146(17) 0.0145(19) C12 0.033(2) 0.059(3) 0.086(4) -0.001(2) 0.020(2) 0.020(3) C13 0.033(2) 0.059(3) 0.096(4) -0.010(2) 0.007(2) 0.005(3) C14 0.036(2) 0.052(2) 0.071(3) -0.015(2) -0.004(2) 0.007(2) C15 0.0329(19) 0.0330(19) 0.047(2) -0.0018(15) -0.0004(16) 0.0034(17) C16 0.0319(18) 0.0290(18) 0.040(2) 0.0031(14) 0.0044(15) 0.0076(15) C17 0.0270(15) 0.0264(16) 0.0279(16) 0.0022(13) 0.0045(12) -0.0035(13) C18 0.037(2) 0.0321(17) 0.039(2) 0.0034(14) 0.0005(15) 0.0015(15) C19 0.041(2) 0.036(2) 0.059(3) 0.0074(16) 0.0006(18) 0.0106(19) C20 0.043(2) 0.0276(18) 0.070(3) 0.0073(16) 0.014(2) 0.0029(19) C21 0.043(2) 0.0295(19) 0.064(3) -0.0002(16) 0.003(2) -0.0094(18) C22 0.038(2) 0.0273(18) 0.047(2) -0.0003(14) -0.0023(16) -0.0066(16) C23 0.0311(16) 0.0241(15) 0.0213(15) 0.0004(12) 0.0019(12) -0.0010(12) C24 0.0297(15) 0.0251(15) 0.0251(15) -0.0003(13) 0.0014(13) -0.0024(13) C25 0.0264(15) 0.0256(16) 0.0265(16) 0.0001(12) 0.0001(12) 0.0025(12) C26 0.0284(16) 0.0324(16) 0.0301(16) 0.0025(14) 0.0030(13) -0.0006(14) C27 0.0232(15) 0.0424(19) 0.0342(18) 0.0026(13) 0.0019(14) 0.0022(16) C28 0.0317(19) 0.049(2) 0.0299(18) 0.0033(15) 0.0058(14) -0.0046(15) C29 0.0317(18) 0.044(2) 0.0270(17) 0.0024(15) 0.0028(14) -0.0069(15) C30 0.0316(16) 0.0300(16) 0.0220(15) 0.0037(12) 0.0000(13) 0.0022(14) C31 0.0255(15) 0.0282(16) 0.0242(15) -0.0005(12) -0.0035(12) 0.0007(13) C32 0.0321(18) 0.047(2) 0.0349(18) -0.0078(15) -0.0054(15) -0.0130(16) Br2 0.0435(2) 0.0550(2) 0.0423(2) -0.00769(19) -0.00983(19) -0.00133(19) O3 0.0301(12) 0.0305(12) 0.0415(14) 0.0025(10) 0.0129(11) -0.0005(11) O4 0.0351(14) 0.0499(16) 0.0415(16) -0.0055(12) 0.0175(12) -0.0080(13) N3 0.0394(17) 0.0342(17) 0.0387(17) 0.0073(13) 0.0039(14) -0.0059(13) N4 0.0492(18) 0.0350(15) 0.0253(14) 0.0036(14) 0.0091(13) 0.0005(12) C33 0.0293(16) 0.0318(17) 0.0274(17) 0.0002(13) 0.0044(13) -0.0012(13) C34 0.0295(16) 0.0280(15) 0.0298(16) -0.0017(13) 0.0078(14) -0.0003(12) C35 0.0337(16) 0.0310(16) 0.0316(16) 0.0022(15) 0.0063(14) 0.0028(13) C36 0.0364(19) 0.0334(18) 0.040(2) 0.0002(14) 0.0039(15) 0.0014(15) C37 0.040(2) 0.058(3) 0.059(3) 0.0083(18) -0.0011(19) -0.009(2) C38 0.066(3) 0.037(2) 0.049(2) 0.011(2) 0.011(2) -0.0114(19) C39 0.043(2) 0.0280(18) 0.0279(17) -0.0008(14) 0.0087(14) 0.0006(14) C40 0.054(3) 0.055(2) 0.036(2) -0.013(2) 0.0160(18) -0.0104(19) C41 0.075(3) 0.066(3) 0.031(2) -0.017(2) 0.013(2) -0.014(2) C42 0.069(3) 0.047(2) 0.031(2) -0.009(2) 0.0019(18) -0.0097(18) C43 0.047(2) 0.0289(17) 0.0348(18) -0.0035(16) -0.0022(15) -0.0009(15) C44 0.048(2) 0.040(2) 0.044(2) -0.0053(17) -0.0108(18) -0.0002(17) C45 0.045(2) 0.042(2) 0.053(3) -0.0093(17) -0.009(2) 0.0095(19) C46 0.0363(19) 0.042(2) 0.039(2) -0.0012(16) 0.0024(16) 0.0106(16) C47 0.0379(17) 0.0302(16) 0.0302(17) -0.0001(16) 0.0023(14) 0.0024(14) C48 0.041(2) 0.0246(16) 0.0305(17) -0.0002(14) 0.0021(14) 0.0027(13) C49 0.0282(16) 0.0276(16) 0.0290(17) -0.0015(13) 0.0010(13) -0.0028(13) C50 0.0339(18) 0.0365(19) 0.039(2) 0.0036(16) 0.0004(15) -0.0022(17) C51 0.045(2) 0.041(2) 0.044(2) 0.0093(18) -0.0049(17) 0.0024(19) C52 0.051(2) 0.043(2) 0.039(2) 0.0023(18) -0.0076(18) 0.0110(17) C53 0.041(2) 0.058(3) 0.039(2) 0.0013(18) 0.0032(16) 0.0168(18) C54 0.0289(18) 0.047(2) 0.037(2) 0.0062(15) 0.0027(14) 0.0085(16) C55 0.0308(16) 0.0248(14) 0.0283(16) 0.0043(13) 0.0044(13) 0.0014(12) C56 0.0375(18) 0.0282(17) 0.0236(16) -0.0006(13) 0.0062(13) -0.0008(13) C57 0.0353(17) 0.0286(16) 0.0234(15) 0.0026(14) 0.0032(13) 0.0040(14) C58 0.0327(18) 0.0343(18) 0.0275(17) 0.0014(13) 0.0011(13) 0.0023(14) C59 0.0399(19) 0.0352(18) 0.0309(17) -0.0005(14) -0.0068(15) 0.0049(16) C60 0.055(2) 0.042(2) 0.0260(17) 0.0029(19) -0.0049(16) -0.0027(15) C61 0.061(3) 0.039(2) 0.0234(17) 0.0043(18) 0.0039(16) -0.0042(15) C62 0.0422(19) 0.0289(16) 0.0250(16) 0.0041(14) 0.0035(15) 0.0022(14) C63 0.0336(17) 0.0299(17) 0.0312(18) 0.0020(14) 0.0080(14) 0.0022(14) C64 0.047(3) 0.070(3) 0.049(3) -0.002(2) 0.030(2) -0.004(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' 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 O1 H1O . . 109.5 ? C31 O2 C32 . . 117.4(3) ? C5 N1 C4 . . 111.0(3) ? C5 N1 C6 . . 110.1(4) ? C4 N1 C6 . . 111.0(3) ? C31 N2 C30 . . 117.1(3) ? C17 C1 C23 . . 109.9(3) ? C17 C1 C2 . . 116.8(3) ? C23 C1 C2 . . 112.2(3) ? C17 C1 H1 . . 105.7 ? C23 C1 H1 . . 105.7 ? C2 C1 H1 . . 105.7 ? O1 C2 C3 . . 106.7(3) ? O1 C2 C7 . . 110.2(3) ? C3 C2 C7 . . 109.0(3) ? O1 C2 C1 . . 107.1(3) ? C3 C2 C1 . . 112.1(3) ? C7 C2 C1 . . 111.7(3) ? C4 C3 C2 . . 112.8(3) ? C4 C3 H3A . . 109.0 ? C2 C3 H3A . . 109.0 ? C4 C3 H3B . . 109.0 ? C2 C3 H3B . . 109.0 ? H3A C3 H3B . . 107.8 ? N1 C4 C3 . . 112.2(3) ? N1 C4 H4A . . 109.2 ? C3 C4 H4A . . 109.2 ? N1 C4 H4B . . 109.2 ? C3 C4 H4B . . 109.2 ? H4A C4 H4B . . 107.9 ? N1 C5 H5A . . 109.5 ? N1 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? N1 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? N1 C6 H6A . . 109.5 ? N1 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? N1 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? C8 C7 C16 . . 118.4(3) ? C8 C7 C2 . . 118.0(3) ? C16 C7 C2 . . 123.2(3) ? C7 C8 C9 . . 122.2(4) ? C7 C8 H8 . . 118.9 ? C9 C8 H8 . . 118.9 ? C10 C9 C8 . . 120.2(4) ? C10 C9 H9 . . 119.9 ? C8 C9 H9 . . 119.9 ? C9 C10 C11 . . 120.9(4) ? C9 C10 H10 . . 119.5 ? C11 C10 H10 . . 119.5 ? C12 C11 C10 . . 120.4(4) ? C12 C11 C16 . . 119.6(4) ? C10 C11 C16 . . 119.9(4) ? C13 C12 C11 . . 121.3(4) ? C13 C12 H12 . . 119.4 ? C11 C12 H12 . . 119.4 ? C12 C13 C14 . . 120.0(4) ? C12 C13 H13 . . 120.0 ? C14 C13 H13 . . 120.0 ? C15 C14 C13 . . 120.7(5) ? C15 C14 H14 . . 119.7 ? C13 C14 H14 . . 119.7 ? C14 C15 C16 . . 121.8(4) ? C14 C15 H15 . . 119.1 ? C16 C15 H15 . . 119.1 ? C15 C16 C11 . . 116.5(4) ? C15 C16 C7 . . 125.3(3) ? C11 C16 C7 . . 118.2(4) ? C22 C17 C18 . . 117.3(3) ? C22 C17 C1 . . 125.2(3) ? C18 C17 C1 . . 117.3(3) ? C19 C18 C17 . . 121.3(4) ? C19 C18 H18 . . 119.4 ? C17 C18 H18 . . 119.4 ? C20 C19 C18 . . 120.5(4) ? C20 C19 H19 . . 119.7 ? C18 C19 H19 . . 119.7 ? C21 C20 C19 . . 118.5(4) ? C21 C20 H20 . . 120.7 ? C19 C20 H20 . . 120.7 ? C20 C21 C22 . . 121.4(4) ? C20 C21 H21 . . 119.3 ? C22 C21 H21 . . 119.3 ? C21 C22 C17 . . 120.9(4) ? C21 C22 H22 . . 119.5 ? C17 C22 H22 . . 119.5 ? C24 C23 C31 . . 116.5(3) ? C24 C23 C1 . . 124.3(3) ? C31 C23 C1 . . 119.2(3) ? C23 C24 C25 . . 120.8(3) ? C23 C24 H24 . . 119.6 ? C25 C24 H24 . . 119.6 ? C26 C25 C30 . . 119.6(3) ? C26 C25 C24 . . 123.1(3) ? C30 C25 C24 . . 117.3(3) ? C27 C26 C25 . . 119.2(3) ? C27 C26 H26 . . 120.4 ? C25 C26 H26 . . 120.4 ? C26 C27 C28 . . 122.2(3) ? C26 C27 Br1 . . 120.1(3) ? C28 C27 Br1 . . 117.7(3) ? C29 C28 C27 . . 119.3(3) ? C29 C28 H28 . . 120.4 ? C27 C28 H28 . . 120.4 ? C28 C29 C30 . . 120.8(3) ? C28 C29 H29 . . 119.6 ? C30 C29 H29 . . 119.6 ? N2 C30 C29 . . 118.5(3) ? N2 C30 C25 . . 122.5(3) ? C29 C30 C25 . . 118.9(3) ? N2 C31 O2 . . 119.0(3) ? N2 C31 C23 . . 125.8(3) ? O2 C31 C23 . . 115.2(3) ? O2 C32 H32A . . 109.5 ? O2 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? O2 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? C34 O3 H3O . . 109.5 ? C63 O4 C64 . . 117.1(3) ? C37 N3 C38 . . 110.1(3) ? C37 N3 C36 . . 111.1(3) ? C38 N3 C36 . . 112.1(3) ? C63 N4 C62 . . 117.5(3) ? C55 C33 C49 . . 108.2(3) ? C55 C33 C34 . . 113.8(3) ? C49 C33 C34 . . 115.8(3) ? C55 C33 H33 . . 106.1 ? C49 C33 H33 . . 106.1 ? C34 C33 H33 . . 106.1 ? O3 C34 C35 . . 106.7(3) ? O3 C34 C39 . . 109.5(3) ? C35 C34 C39 . . 111.8(3) ? O3 C34 C33 . . 107.0(3) ? C35 C34 C33 . . 111.3(3) ? C39 C34 C33 . . 110.3(3) ? C36 C35 C34 . . 112.8(3) ? C36 C35 H35A . . 109.0 ? C34 C35 H35A . . 109.0 ? C36 C35 H35B . . 109.0 ? C34 C35 H35B . . 109.0 ? H35A C35 H35B . . 107.8 ? N3 C36 C35 . . 110.5(3) ? N3 C36 H36A . . 109.5 ? C35 C36 H36A . . 109.5 ? N3 C36 H36B . . 109.5 ? C35 C36 H36B . . 109.5 ? H36A C36 H36B . . 108.1 ? N3 C37 H37A . . 109.5 ? N3 C37 H37B . . 109.5 ? H37A C37 H37B . . 109.5 ? N3 C37 H37C . . 109.5 ? H37A C37 H37C . . 109.5 ? H37B C37 H37C . . 109.5 ? N3 C38 H38A . . 109.5 ? N3 C38 H38B . . 109.5 ? H38A C38 H38B . . 109.5 ? N3 C38 H38C . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? C40 C39 C48 . . 118.0(4) ? C40 C39 C34 . . 117.9(3) ? C48 C39 C34 . . 124.1(3) ? C39 C40 C41 . . 123.2(4) ? C39 C40 H40 . . 118.4 ? C41 C40 H40 . . 118.4 ? C42 C41 C40 . . 120.1(4) ? C42 C41 H41 . . 119.9 ? C40 C41 H41 . . 119.9 ? C41 C42 C43 . . 120.0(4) ? C41 C42 H42 . . 120.0 ? C43 C42 H42 . . 120.0 ? C42 C43 C44 . . 119.8(4) ? C42 C43 C48 . . 120.5(4) ? C44 C43 C48 . . 119.7(4) ? C45 C44 C43 . . 121.3(4) ? C45 C44 H44 . . 119.3 ? C43 C44 H44 . . 119.3 ? C44 C45 C46 . . 119.6(4) ? C44 C45 H45 . . 120.2 ? C46 C45 H45 . . 120.2 ? C47 C46 C45 . . 120.7(4) ? C47 C46 H46 . . 119.7 ? C45 C46 H46 . . 119.7 ? C46 C47 C48 . . 122.1(4) ? C46 C47 H47 . . 119.0 ? C48 C47 H47 . . 119.0 ? C47 C48 C43 . . 116.5(3) ? C47 C48 C39 . . 125.5(3) ? C43 C48 C39 . . 118.0(3) ? C50 C49 C54 . . 117.9(3) ? C50 C49 C33 . . 117.6(3) ? C54 C49 C33 . . 124.2(3) ? C49 C50 C51 . . 122.0(4) ? C49 C50 H50 . . 119.0 ? C51 C50 H50 . . 119.0 ? C52 C51 C50 . . 119.6(4) ? C52 C51 H51 . . 120.2 ? C50 C51 H51 . . 120.2 ? C51 C52 C53 . . 119.7(4) ? C51 C52 H52 . . 120.1 ? C53 C52 H52 . . 120.1 ? C52 C53 C54 . . 120.4(4) ? C52 C53 H53 . . 119.8 ? C54 C53 H53 . . 119.8 ? C53 C54 C49 . . 120.3(3) ? C53 C54 H54 . . 119.8 ? C49 C54 H54 . . 119.8 ? C56 C55 C63 . . 116.2(3) ? C56 C55 C33 . . 123.8(3) ? C63 C55 C33 . . 119.8(3) ? C55 C56 C57 . . 121.2(3) ? C55 C56 H56 . . 119.4 ? C57 C56 H56 . . 119.4 ? C58 C57 C62 . . 119.9(3) ? C58 C57 C56 . . 123.2(3) ? C62 C57 C56 . . 116.9(3) ? C59 C58 C57 . . 119.6(3) ? C59 C58 H58 . . 120.2 ? C57 C58 H58 . . 120.2 ? C58 C59 C60 . . 121.7(4) ? C58 C59 Br2 . . 119.5(3) ? C60 C59 Br2 . . 118.8(3) ? C61 C60 C59 . . 119.1(4) ? C61 C60 H60 . . 120.4 ? C59 C60 H60 . . 120.4 ? C60 C61 C62 . . 121.2(4) ? C60 C61 H61 . . 119.4 ? C62 C61 H61 . . 119.4 ? N4 C62 C61 . . 119.3(3) ? N4 C62 C57 . . 122.3(3) ? C61 C62 C57 . . 118.4(4) ? N4 C63 O4 . . 119.4(3) ? N4 C63 C55 . . 125.7(3) ? O4 C63 C55 . . 114.9(3) ? O4 C64 H64A . . 109.5 ? O4 C64 H64B . . 109.5 ? H64A C64 H64B . . 109.5 ? O4 C64 H64C . . 109.5 ? H64A C64 H64C . . 109.5 ? H64B C64 H64C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C27 . 1.903(3) ? O1 C2 . 1.421(4) ? O1 H1O . 0.8400 ? O2 C31 . 1.354(4) ? O2 C32 . 1.437(4) ? N1 C5 . 1.461(5) ? N1 C4 . 1.470(5) ? N1 C6 . 1.477(5) ? N2 C31 . 1.311(4) ? N2 C30 . 1.372(4) ? C1 C17 . 1.526(4) ? C1 C23 . 1.531(4) ? C1 C2 . 1.560(5) ? C1 H1 . 1.0000 ? C2 C3 . 1.545(5) ? C2 C7 . 1.550(5) ? C3 C4 . 1.530(5) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? C7 C8 . 1.377(5) ? C7 C16 . 1.449(5) ? C8 C9 . 1.417(5) ? C8 H8 . 0.9500 ? C9 C10 . 1.346(7) ? C9 H9 . 0.9500 ? C10 C11 . 1.413(6) ? C10 H10 . 0.9500 ? C11 C12 . 1.404(7) ? C11 C16 . 1.438(5) ? C12 C13 . 1.366(8) ? C12 H12 . 0.9500 ? C13 C14 . 1.384(7) ? C13 H13 . 0.9500 ? C14 C15 . 1.371(6) ? C14 H14 . 0.9500 ? C15 C16 . 1.420(6) ? C15 H15 . 0.9500 ? C17 C22 . 1.391(5) ? C17 C18 . 1.395(5) ? C18 C19 . 1.388(5) ? C18 H18 . 0.9500 ? C19 C20 . 1.382(6) ? C19 H19 . 0.9500 ? C20 C21 . 1.372(6) ? C20 H20 . 0.9500 ? C21 C22 . 1.385(5) ? C21 H21 . 0.9500 ? C22 H22 . 0.9500 ? C23 C24 . 1.361(5) ? C23 C31 . 1.435(4) ? C24 C25 . 1.424(4) ? C24 H24 . 0.9500 ? C25 C26 . 1.416(5) ? C25 C30 . 1.421(5) ? C26 C27 . 1.365(5) ? C26 H26 . 0.9500 ? C27 C28 . 1.409(5) ? C28 C29 . 1.369(5) ? C28 H28 . 0.9500 ? C29 C30 . 1.418(5) ? C29 H29 . 0.9500 ? C32 H32A . 0.9800 ? C32 H32B . 0.9800 ? C32 H32C . 0.9800 ? Br2 C59 . 1.902(4) ? O3 C34 . 1.435(4) ? O3 H3O . 0.8400 ? O4 C63 . 1.358(4) ? O4 C64 . 1.443(4) ? N3 C37 . 1.460(6) ? N3 C38 . 1.464(5) ? N3 C36 . 1.482(5) ? N4 C63 . 1.305(5) ? N4 C62 . 1.374(5) ? C33 C55 . 1.526(5) ? C33 C49 . 1.531(5) ? C33 C34 . 1.552(5) ? C33 H33 . 1.0000 ? C34 C35 . 1.546(5) ? C34 C39 . 1.550(5) ? C35 C36 . 1.524(5) ? C35 H35A . 0.9900 ? C35 H35B . 0.9900 ? C36 H36A . 0.9900 ? C36 H36B . 0.9900 ? C37 H37A . 0.9800 ? C37 H37B . 0.9800 ? C37 H37C . 0.9800 ? C38 H38A . 0.9800 ? C38 H38B . 0.9800 ? C38 H38C . 0.9800 ? C39 C40 . 1.365(5) ? C39 C48 . 1.443(5) ? C40 C41 . 1.409(6) ? C40 H40 . 0.9500 ? C41 C42 . 1.347(7) ? C41 H41 . 0.9500 ? C42 C43 . 1.412(6) ? C42 H42 . 0.9500 ? C43 C44 . 1.416(6) ? C43 C48 . 1.436(5) ? C44 C45 . 1.360(6) ? C44 H44 . 0.9500 ? C45 C46 . 1.407(6) ? C45 H45 . 0.9500 ? C46 C47 . 1.362(5) ? C46 H46 . 0.9500 ? C47 C48 . 1.425(5) ? C47 H47 . 0.9500 ? C49 C50 . 1.378(5) ? C49 C54 . 1.402(5) ? C50 C51 . 1.390(6) ? C50 H50 . 0.9500 ? C51 C52 . 1.376(6) ? C51 H51 . 0.9500 ? C52 C53 . 1.385(6) ? C52 H52 . 0.9500 ? C53 C54 . 1.393(5) ? C53 H53 . 0.9500 ? C54 H54 . 0.9500 ? C55 C56 . 1.362(5) ? C55 C63 . 1.435(5) ? C56 C57 . 1.426(5) ? C56 H56 . 0.9500 ? C57 C58 . 1.400(5) ? C57 C62 . 1.423(5) ? C58 C59 . 1.367(5) ? C58 H58 . 0.9500 ? C59 C60 . 1.406(6) ? C60 C61 . 1.371(6) ? C60 H60 . 0.9500 ? C61 C62 . 1.409(5) ? C61 H61 . 0.9500 ? C64 H64A . 0.9800 ? C64 H64B . 0.9800 ? C64 H64C . 0.9800 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H1O N1 . 0.84 1.94 2.696(4) 150.0 yes C1 H1 O2 . 1.00 2.24 2.763(4) 111.1 yes O3 H3O N3 . 0.84 1.93 2.685(4) 149.1 yes C33 H33 O4 . 1.00 2.23 2.773(4) 112.4 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C17 C1 C2 O1 . . . . 52.3(4) ? C23 C1 C2 O1 . . . . -75.9(3) ? C17 C1 C2 C3 . . . . 169.0(3) ? C23 C1 C2 C3 . . . . 40.8(4) ? C17 C1 C2 C7 . . . . -68.4(4) ? C23 C1 C2 C7 . . . . 163.4(3) ? O1 C2 C3 C4 . . . . -67.4(3) ? C7 C2 C3 C4 . . . . 51.6(4) ? C1 C2 C3 C4 . . . . 175.7(3) ? C5 N1 C4 C3 . . . . 83.1(4) ? C6 N1 C4 C3 . . . . -154.1(3) ? C2 C3 C4 N1 . . . . 58.7(4) ? O1 C2 C7 C8 . . . . -0.5(4) ? C3 C2 C7 C8 . . . . -117.3(3) ? C1 C2 C7 C8 . . . . 118.3(3) ? O1 C2 C7 C16 . . . . 171.3(3) ? C3 C2 C7 C16 . . . . 54.5(4) ? C1 C2 C7 C16 . . . . -69.8(4) ? C16 C7 C8 C9 . . . . -2.8(5) ? C2 C7 C8 C9 . . . . 169.4(3) ? C7 C8 C9 C10 . . . . -0.8(6) ? C8 C9 C10 C11 . . . . 2.5(6) ? C9 C10 C11 C12 . . . . 178.7(4) ? C9 C10 C11 C16 . . . . -0.6(6) ? C10 C11 C12 C13 . . . . -176.8(5) ? C16 C11 C12 C13 . . . . 2.4(7) ? C11 C12 C13 C14 . . . . -0.7(8) ? C12 C13 C14 C15 . . . . -1.2(8) ? C13 C14 C15 C16 . . . . 1.5(7) ? C14 C15 C16 C11 . . . . 0.2(6) ? C14 C15 C16 C7 . . . . -179.7(4) ? C12 C11 C16 C15 . . . . -2.1(6) ? C10 C11 C16 C15 . . . . 177.2(4) ? C12 C11 C16 C7 . . . . 177.8(4) ? C10 C11 C16 C7 . . . . -2.9(5) ? C8 C7 C16 C15 . . . . -175.6(4) ? C2 C7 C16 C15 . . . . 12.6(6) ? C8 C7 C16 C11 . . . . 4.6(5) ? C2 C7 C16 C11 . . . . -167.3(3) ? C23 C1 C17 C22 . . . . 81.5(4) ? C2 C1 C17 C22 . . . . -47.9(5) ? C23 C1 C17 C18 . . . . -93.4(4) ? C2 C1 C17 C18 . . . . 137.3(3) ? C22 C17 C18 C19 . . . . -1.0(6) ? C1 C17 C18 C19 . . . . 174.2(4) ? C17 C18 C19 C20 . . . . 0.5(6) ? C18 C19 C20 C21 . . . . 0.1(7) ? C19 C20 C21 C22 . . . . -0.1(7) ? C20 C21 C22 C17 . . . . -0.4(7) ? C18 C17 C22 C21 . . . . 0.9(6) ? C1 C17 C22 C21 . . . . -173.9(4) ? C17 C1 C23 C24 . . . . -54.5(4) ? C2 C1 C23 C24 . . . . 77.3(4) ? C17 C1 C23 C31 . . . . 126.0(3) ? C2 C1 C23 C31 . . . . -102.2(3) ? C31 C23 C24 C25 . . . . -0.6(5) ? C1 C23 C24 C25 . . . . 179.8(3) ? C23 C24 C25 C26 . . . . 178.3(3) ? C23 C24 C25 C30 . . . . -1.1(5) ? C30 C25 C26 C27 . . . . 0.1(5) ? C24 C25 C26 C27 . . . . -179.3(3) ? C25 C26 C27 C28 . . . . 0.1(5) ? C25 C26 C27 Br1 . . . . -180.0(3) ? C26 C27 C28 C29 . . . . -0.3(6) ? Br1 C27 C28 C29 . . . . 179.8(3) ? C27 C28 C29 C30 . . . . 0.2(6) ? C31 N2 C30 C29 . . . . -177.9(3) ? C31 N2 C30 C25 . . . . -0.3(5) ? C28 C29 C30 N2 . . . . 177.8(3) ? C28 C29 C30 C25 . . . . 0.0(5) ? C26 C25 C30 N2 . . . . -177.8(3) ? C24 C25 C30 N2 . . . . 1.6(5) ? C26 C25 C30 C29 . . . . -0.2(5) ? C24 C25 C30 C29 . . . . 179.3(3) ? C30 N2 C31 O2 . . . . 176.5(3) ? C30 N2 C31 C23 . . . . -1.7(5) ? C32 O2 C31 N2 . . . . 0.6(5) ? C32 O2 C31 C23 . . . . 179.0(3) ? C24 C23 C31 N2 . . . . 2.1(5) ? C1 C23 C31 N2 . . . . -178.3(3) ? C24 C23 C31 O2 . . . . -176.1(3) ? C1 C23 C31 O2 . . . . 3.5(4) ? C55 C33 C34 O3 . . . . -63.8(3) ? C49 C33 C34 O3 . . . . 62.5(4) ? C55 C33 C34 C35 . . . . 52.5(4) ? C49 C33 C34 C35 . . . . 178.8(3) ? C55 C33 C34 C39 . . . . 177.2(3) ? C49 C33 C34 C39 . . . . -56.5(4) ? O3 C34 C35 C36 . . . . -66.6(4) ? C39 C34 C35 C36 . . . . 53.1(4) ? C33 C34 C35 C36 . . . . 177.0(3) ? C37 N3 C36 C35 . . . . 84.3(4) ? C38 N3 C36 C35 . . . . -152.0(3) ? C34 C35 C36 N3 . . . . 63.0(4) ? O3 C34 C39 C40 . . . . -5.9(5) ? C35 C34 C39 C40 . . . . -123.9(4) ? C33 C34 C39 C40 . . . . 111.6(4) ? O3 C34 C39 C48 . . . . 171.9(3) ? C35 C34 C39 C48 . . . . 53.8(4) ? C33 C34 C39 C48 . . . . -70.7(4) ? C48 C39 C40 C41 . . . . -1.6(7) ? C34 C39 C40 C41 . . . . 176.3(4) ? C39 C40 C41 C42 . . . . -1.6(8) ? C40 C41 C42 C43 . . . . 1.5(8) ? C41 C42 C43 C44 . . . . -179.2(5) ? C41 C42 C43 C48 . . . . 1.6(7) ? C42 C43 C44 C45 . . . . -178.0(4) ? C48 C43 C44 C45 . . . . 1.2(6) ? C43 C44 C45 C46 . . . . 1.5(6) ? C44 C45 C46 C47 . . . . -2.5(6) ? C45 C46 C47 C48 . . . . 0.8(6) ? C46 C47 C48 C43 . . . . 1.9(5) ? C46 C47 C48 C39 . . . . -177.0(3) ? C42 C43 C48 C47 . . . . 176.4(4) ? C44 C43 C48 C47 . . . . -2.8(5) ? C42 C43 C48 C39 . . . . -4.7(5) ? C44 C43 C48 C39 . . . . 176.2(3) ? C40 C39 C48 C47 . . . . -176.6(4) ? C34 C39 C48 C47 . . . . 5.7(5) ? C40 C39 C48 C43 . . . . 4.5(5) ? C34 C39 C48 C43 . . . . -173.2(3) ? C55 C33 C49 C50 . . . . -91.5(4) ? C34 C33 C49 C50 . . . . 139.4(3) ? C55 C33 C49 C54 . . . . 82.5(4) ? C34 C33 C49 C54 . . . . -46.6(5) ? C54 C49 C50 C51 . . . . -0.6(6) ? C33 C49 C50 C51 . . . . 173.8(4) ? C49 C50 C51 C52 . . . . 0.8(6) ? C50 C51 C52 C53 . . . . -0.5(7) ? C51 C52 C53 C54 . . . . -0.1(7) ? C52 C53 C54 C49 . . . . 0.4(6) ? C50 C49 C54 C53 . . . . 0.0(6) ? C33 C49 C54 C53 . . . . -174.0(4) ? C49 C33 C55 C56 . . . . -63.1(4) ? C34 C33 C55 C56 . . . . 67.1(4) ? C49 C33 C55 C63 . . . . 112.6(3) ? C34 C33 C55 C63 . . . . -117.2(3) ? C63 C55 C56 C57 . . . . -2.4(5) ? C33 C55 C56 C57 . . . . 173.4(3) ? C55 C56 C57 C58 . . . . 179.8(3) ? C55 C56 C57 C62 . . . . -2.1(5) ? C62 C57 C58 C59 . . . . -1.7(5) ? C56 C57 C58 C59 . . . . 176.3(3) ? C57 C58 C59 C60 . . . . -0.8(5) ? C57 C58 C59 Br2 . . . . 180.0(3) ? C58 C59 C60 C61 . . . . 1.7(6) ? Br2 C59 C60 C61 . . . . -179.1(3) ? C59 C60 C61 C62 . . . . -0.1(6) ? C63 N4 C62 C61 . . . . 177.2(3) ? C63 N4 C62 C57 . . . . -2.6(5) ? C60 C61 C62 N4 . . . . 177.9(3) ? C60 C61 C62 C57 . . . . -2.4(5) ? C58 C57 C62 N4 . . . . -177.0(3) ? C56 C57 C62 N4 . . . . 4.8(5) ? C58 C57 C62 C61 . . . . 3.3(5) ? C56 C57 C62 C61 . . . . -174.9(3) ? C62 N4 C63 O4 . . . . 178.1(3) ? C62 N4 C63 C55 . . . . -2.6(5) ? C64 O4 C63 N4 . . . . -0.1(5) ? C64 O4 C63 C55 . . . . -179.4(3) ? C56 C55 C63 N4 . . . . 5.1(5) ? C33 C55 C63 N4 . . . . -170.9(3) ? C56 C55 C63 O4 . . . . -175.6(3) ? C33 C55 C63 O4 . . . . 8.4(5) ? _cod_database_fobs_code 2022265