#------------------------------------------------------------------------------ #$Date: 2024-11-22 01:06:07 +0200 (Fri, 22 Nov 2024) $ #$Revision: 296050 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573250.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_1573250 loop_ _publ_author_name 'Navaneetha, N.' 'Maurya, Sundaram' 'Behera, Prativa' 'Jadhav, Sandip B.' 'Magham, Lakshmi Revati' 'Nanubolu, Jagadeesh Babu' 'Roy, Lisa' 'Chegondi, Rambabu' _publ_section_title ; BINAP-CuH-catalysed enantioselective allylation using alkoxyallenes to access 1,2-syn-tert,sec-diols ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07002J _journal_year 2024 _chemical_formula_moiety 'C23 H21 Br2 N O2' _chemical_formula_sum 'C23 H21 Br2 N O2' _chemical_formula_weight 503.23 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/3 _audit_update_record ; 2024-04-21 deposited with the CCDC. 2024-11-04 downloaded from the CCDC. ; _cell_angle_alpha 73.632(7) _cell_angle_beta 82.000(11) _cell_angle_gamma 75.587(7) _cell_formula_units_Z 2 _cell_length_a 8.759(2) _cell_length_b 8.907(3) _cell_length_c 15.126(5) _cell_measurement_reflns_used 5415 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 22.235 _cell_measurement_theta_min 2.405 _cell_volume 1093.6(6) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON III C7 HPAD' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_unetI/netI 0.0725 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 18857 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.399 _diffrn_reflns_theta_min 2.407 _diffrn_source microfocus _exptl_absorpt_coefficient_mu 3.724 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5312 _exptl_absorpt_correction_type multi-scan _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_crystal_density_diffrn 1.528 _exptl_crystal_description BLOCK _exptl_crystal_F_000 504 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM/hexane (1:9)' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.722 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 257 _refine_ls_number_reflns 4431 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0484 _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^)+(0.0297P)^2^+1.0853P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0940 _refine_ls_wR_factor_ref 0.1115 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2743 _reflns_number_total 4431 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07002j2.cif _cod_data_source_block KB378_0m _cod_database_code 1573250 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.481 _shelx_estimated_absorpt_t_max 0.664 _shelx_res_file ; TITL KB378_0m_a.res in P-1 KB378_0m.res created by SHELXL-2019/3 at 14:23:45 on 20-Apr-2024 CELL 0.71073 8.7593 8.9068 15.1261 73.632 82.000 75.587 ZERR 2.00 0.0023 0.0031 0.0051 0.007 0.011 0.007 LATT 1 SFAC C H N O BR UNIT 46 42 2 4 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 21 ACTA L.S. 40 FMAP 2 PLAN 5 OMIT -3 55 OMIT 0 1 5 OMIT 0 1 4 OMIT 0 1 3 OMIT 0 0 1 HTAB BOND $H SIZE 0.23 0.14 0.12 CONF WGHT 0.029700 1.085300 FVAR 0.94850 BR1 5 0.719463 0.254965 0.458464 11.00000 0.12120 0.07371 = 0.06087 -0.03304 -0.01646 -0.01745 BR2 5 0.047232 1.151478 0.671326 11.00000 0.06805 0.07036 = 0.08886 -0.00988 -0.00551 0.01985 O1 4 0.697414 0.578554 0.820342 11.00000 0.04689 0.04009 = 0.03919 -0.00639 -0.01494 -0.00263 O2 4 0.750970 0.429617 1.002582 11.00000 0.05232 0.06894 = 0.04423 -0.02449 -0.01461 -0.00036 H2O 2 0.662101 0.469194 0.996389 11.00000 -1.50000 N1 3 0.530428 0.321389 0.949069 11.00000 0.04681 0.05133 = 0.05843 -0.01457 -0.00637 -0.00774 C1 1 0.690420 0.672668 0.727211 11.00000 0.04362 0.03902 = 0.03984 -0.00786 -0.00778 -0.01027 AFIX 13 H1 2 0.778832 0.726955 0.711243 11.00000 -1.20000 AFIX 0 C2 1 0.537048 0.797401 0.720243 11.00000 0.04758 0.03160 = 0.03997 -0.01017 -0.00845 -0.01042 C3 1 0.408629 0.776740 0.783227 11.00000 0.05672 0.04285 = 0.04081 -0.00253 -0.00434 -0.00801 AFIX 43 H3 2 0.419680 0.690080 0.835185 11.00000 -1.20000 AFIX 0 C4 1 0.264775 0.882818 0.769944 11.00000 0.05133 0.05379 = 0.05078 -0.01279 0.00370 -0.00665 AFIX 43 H4 2 0.178821 0.867418 0.812376 11.00000 -1.20000 AFIX 0 C5 1 0.248775 1.011769 0.693564 11.00000 0.05770 0.04062 = 0.04882 -0.01484 -0.00624 0.00069 C6 1 0.375642 1.038343 0.631724 11.00000 0.06444 0.03499 = 0.04270 -0.00158 -0.00855 -0.00381 AFIX 43 H6 2 0.364986 1.127522 0.581176 11.00000 -1.20000 AFIX 0 C7 1 0.518533 0.931394 0.645543 11.00000 0.05451 0.03896 = 0.04351 -0.00493 -0.00334 -0.01229 AFIX 43 H7 2 0.604838 0.949228 0.603862 11.00000 -1.20000 AFIX 0 C8 1 0.699281 0.571484 0.660214 11.00000 0.03630 0.03946 = 0.03665 -0.00446 -0.01120 -0.00491 C9 1 0.788572 0.594721 0.577018 11.00000 0.04689 0.04107 = 0.04892 -0.00566 -0.00667 -0.00680 AFIX 43 H9 2 0.847639 0.673165 0.561720 11.00000 -1.20000 AFIX 0 C10 1 0.792348 0.504462 0.516015 11.00000 0.05481 0.05415 = 0.03884 -0.01340 0.00096 -0.00509 AFIX 43 H10 2 0.851379 0.523596 0.459545 11.00000 -1.20000 AFIX 0 C11 1 0.708299 0.385984 0.539184 11.00000 0.05956 0.04685 = 0.04240 -0.01390 -0.01961 -0.00081 C12 1 0.617439 0.360059 0.621528 11.00000 0.06427 0.05342 = 0.05088 -0.01276 -0.01204 -0.02148 AFIX 43 H12 2 0.560155 0.280105 0.637033 11.00000 -1.20000 AFIX 0 C13 1 0.612359 0.454023 0.680744 11.00000 0.05402 0.05547 = 0.04081 -0.01324 -0.00334 -0.01845 AFIX 43 H13 2 0.549077 0.438218 0.735800 11.00000 -1.20000 AFIX 0 C14 1 0.840802 0.461342 0.840353 11.00000 0.04061 0.04402 = 0.04805 -0.01395 -0.01696 -0.00426 AFIX 13 H14 2 0.866681 0.402262 0.792556 11.00000 -1.20000 AFIX 0 C15 1 0.974153 0.537312 0.840413 11.00000 0.05882 0.06722 = 0.06965 -0.01807 -0.02134 -0.01858 AFIX 43 H15 2 0.966156 0.597729 0.882638 11.00000 -1.20000 AFIX 0 C16 1 1.100209 0.524050 0.785178 11.00000 0.06665 0.09866 = 0.10406 -0.00891 -0.01605 -0.04058 AFIX 93 H16A 2 1.111382 0.464356 0.742249 11.00000 -1.20000 H16B 2 1.179886 0.574185 0.788297 11.00000 -1.20000 AFIX 0 C17 1 0.804481 0.344447 0.933403 11.00000 0.04862 0.04593 = 0.03951 -0.01311 -0.01103 -0.00066 C18 1 0.955226 0.224108 0.966493 11.00000 0.05727 0.06065 = 0.05979 -0.00909 -0.01888 0.00688 AFIX 137 H18A 2 1.007160 0.175977 0.917767 11.00000 -1.50000 H18B 2 0.929247 0.142303 1.019122 11.00000 -1.50000 H18C 2 1.024282 0.278198 0.983445 11.00000 -1.50000 AFIX 0 C19 1 0.678752 0.262723 0.920589 11.00000 0.05669 0.04045 = 0.03636 -0.00340 -0.00825 -0.00678 C20 1 0.715809 0.137187 0.878684 11.00000 0.07166 0.05382 = 0.05728 -0.02014 0.00156 -0.01326 AFIX 43 H20 2 0.820295 0.096326 0.860682 11.00000 -1.20000 AFIX 0 C21 1 0.596140 0.073296 0.863896 11.00000 0.10657 0.05901 = 0.06910 -0.02900 -0.00025 -0.03190 AFIX 43 H21 2 0.618776 -0.010551 0.835499 11.00000 -1.20000 AFIX 0 C22 1 0.444935 0.134843 0.891472 11.00000 0.08609 0.07495 = 0.08704 -0.02231 -0.01127 -0.03577 AFIX 43 H22 2 0.361977 0.094798 0.881778 11.00000 -1.20000 AFIX 0 C23 1 0.417261 0.256468 0.933635 11.00000 0.05971 0.06535 = 0.08064 -0.01537 -0.00376 -0.01871 AFIX 43 H23 2 0.313411 0.297006 0.952917 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KB378_0m_a.res in P-1 REM wR2 = 0.1115, GooF = S = 1.004, Restrained GooF = 1.004 for all data REM R1 = 0.0484 for 2743 Fo > 4sig(Fo) and 0.0971 for all 4431 data REM 257 parameters refined using 0 restraints END WGHT 0.0297 1.0854 REM Instructions for potential hydrogen bonds HTAB O2 N1 EQIV $1 -x+1, -y+1, -z+2 HTAB O2 N1_$1 HTAB C23 O2_$1 REM Highest difference peak 0.722, deepest hole -0.524, 1-sigma level 0.061 Q1 1 0.8062 0.1940 0.4872 11.00000 0.05 0.72 Q2 1 0.1216 1.1523 0.7103 11.00000 0.05 0.48 Q3 1 0.7610 0.3365 0.4166 11.00000 0.05 0.47 Q4 1 0.6800 0.2547 0.4680 11.00000 0.05 0.40 Q5 1 -0.0066 1.0548 0.6966 11.00000 0.05 0.37 ; _shelx_res_checksum 86794 _shelx_hkl_file ; -1 0 0 382.03 29.26 -1 0 0 412.19 28.98 -1 0 0 408.80 29.00 -1 0 0 417.01 28.97 1 0 0 369.64 28.95 -2 0 0 1410.16 104.93 -2 0 0 1472.92 104.40 -2 0 0 1478.60 104.92 2 0 0 1412.37 104.41 2 0 0 1441.98 105.09 2 0 0 1442.97 104.95 -3 0 0 4211.78 293.14 3 0 0 3894.01 293.28 -4 0 0 2316.68 185.27 -4 0 0 2702.51 185.36 -4 0 0 2681.92 186.53 -4 0 0 2557.26 186.41 4 0 0 2481.54 187.07 4 0 0 2578.02 186.55 4 0 0 2497.10 185.37 4 0 0 2682.57 185.53 -5 0 0 168.68 18.72 -5 0 0 201.09 16.97 -5 0 0 195.87 16.76 -5 0 0 140.80 19.81 -5 0 0 191.09 17.45 5 0 0 160.54 17.11 5 0 0 167.42 22.45 5 0 0 198.32 17.82 5 0 0 158.50 19.47 -6 0 0 165.26 19.47 -6 0 0 164.46 21.25 -6 0 0 193.97 18.88 -6 0 0 152.49 16.28 6 0 0 177.52 17.59 6 0 0 129.51 22.57 6 0 0 197.40 22.79 6 0 0 139.80 17.77 -7 0 0 14.72 12.23 -7 0 0 20.44 15.66 -7 0 0 25.30 7.13 -7 0 0 5.99 15.98 7 0 0 34.52 12.76 7 0 0 51.79 13.97 7 0 0 36.69 14.45 7 0 0 12.18 19.86 -8 0 0 141.59 22.25 -8 0 0 131.88 22.37 8 0 0 94.12 29.77 8 0 0 114.40 18.51 8 0 0 115.92 20.19 -9 0 0 139.99 27.16 -9 0 0 134.74 22.09 9 0 0 143.95 22.45 9 0 0 95.45 22.56 -10 0 0 -15.34 28.06 -10 0 0 25.70 21.77 10 0 0 10.83 21.09 10 0 0 27.67 21.79 10 -1 0 -12.55 19.73 10 -1 0 0.89 22.95 -10 1 0 82.08 23.98 -10 1 0 -24.77 24.84 9 -1 0 15.19 14.26 9 -1 0 -4.82 19.61 -9 1 0 22.96 20.66 -9 1 0 29.35 26.25 8 -1 0 26.45 17.32 -8 1 0 -1.63 23.74 -8 1 0 9.96 17.95 7 -1 0 76.79 13.24 7 -1 0 87.89 16.97 7 -1 0 81.46 24.18 -7 1 0 69.08 14.63 -7 1 0 93.44 19.20 -7 1 0 85.47 23.02 6 -1 0 177.82 24.22 6 -1 0 216.28 21.29 6 -1 0 196.57 26.66 6 -1 0 184.98 20.42 -6 1 0 238.71 26.84 -6 1 0 206.68 20.60 -6 1 0 235.40 25.33 -6 1 0 203.23 20.34 5 -1 0 218.27 23.61 5 -1 0 184.91 19.75 5 -1 0 174.92 24.12 5 -1 0 237.13 20.57 5 -1 0 191.33 18.57 -5 1 0 218.95 19.27 -5 1 0 221.86 22.23 -5 1 0 199.65 22.48 -5 1 0 182.76 19.05 4 -1 0 176.87 22.27 4 -1 0 212.70 18.15 4 -1 0 221.26 19.36 4 -1 0 214.52 18.80 4 -1 0 235.32 22.01 -4 1 0 203.26 18.52 -4 1 0 230.43 21.78 -4 1 0 207.21 21.64 -4 1 0 205.24 18.52 3 -1 0 4970.19 359.86 0 -1 0 759.68 52.24 0 -1 0 652.75 52.11 0 1 0 745.54 52.18 -2 -1 0 633.34 44.47 -2 -1 0 627.11 44.61 -2 -1 0 622.98 44.87 -2 -1 0 614.66 44.79 -2 -1 0 648.05 44.66 -2 -1 0 634.44 44.93 2 1 0 576.87 44.99 2 1 0 603.21 44.38 2 1 0 611.01 44.66 2 1 0 552.45 44.76 -3 -1 0 2611.58 183.62 -3 -1 0 2596.09 183.28 -3 -1 0 2522.29 183.39 3 1 0 2735.88 183.62 3 1 0 2415.30 183.08 3 1 0 2335.42 183.60 -4 -1 0 -8.68 5.96 -4 -1 0 -0.15 5.06 -4 -1 0 -3.20 3.51 -4 -1 0 -14.59 7.35 -4 -1 0 -5.20 6.86 4 1 0 0.75 8.40 4 1 0 4.07 8.76 4 1 0 -4.78 7.26 4 1 0 -10.09 5.52 4 1 0 -1.72 6.51 -5 -1 0 14.21 10.04 -5 -1 0 12.77 6.22 -5 -1 0 30.89 8.13 -5 -1 0 16.03 7.20 -5 -1 0 17.74 5.55 -5 -1 0 5.93 9.46 5 1 0 13.87 12.07 5 1 0 16.97 7.99 5 1 0 14.63 11.20 5 1 0 27.00 10.08 -6 -1 0 969.98 68.52 -6 -1 0 930.79 65.66 -6 -1 0 923.89 66.44 -6 -1 0 914.41 68.60 6 1 0 821.83 69.93 6 1 0 809.81 68.49 6 1 0 881.78 67.39 6 1 0 886.40 67.08 6 1 0 869.04 67.72 -7 -1 0 446.71 38.80 -7 -1 0 429.55 35.74 -7 -1 0 434.32 34.12 -7 -1 0 457.85 40.19 -7 -1 0 485.24 36.66 7 1 0 486.11 38.10 7 1 0 404.62 40.03 7 1 0 415.55 37.57 7 1 0 457.12 44.11 7 1 0 435.05 38.49 -8 -1 0 35.68 16.60 -8 -1 0 2.03 17.53 8 1 0 -28.64 16.21 8 1 0 -5.74 15.05 -9 -1 0 84.64 19.44 -9 -1 0 19.35 19.82 9 1 0 21.64 20.07 9 1 0 30.88 14.67 -10 -1 0 144.68 23.88 10 1 0 83.52 24.34 10 1 0 130.46 25.12 9 -2 0 79.58 24.98 -9 2 0 110.23 26.68 -9 2 0 147.94 29.96 8 -2 0 121.31 21.33 -8 2 0 157.78 28.10 -8 2 0 104.66 24.96 7 -2 0 62.16 18.17 7 -2 0 44.79 15.15 -7 2 0 48.09 21.99 -7 2 0 66.58 20.76 -7 2 0 12.13 13.34 6 -2 0 593.59 45.96 6 -2 0 597.38 46.10 6 -2 0 489.23 52.87 6 -2 0 651.76 48.00 -6 2 0 553.04 46.05 -6 2 0 537.19 45.98 -6 2 0 598.80 51.94 -6 2 0 621.57 50.72 5 -2 0 1789.73 121.50 5 -2 0 1716.91 121.71 5 -2 0 1746.93 122.39 5 -2 0 1464.70 123.72 -5 2 0 1590.97 121.91 -5 2 0 1651.40 122.19 -5 2 0 1653.68 124.18 -5 2 0 1625.64 124.60 4 -2 0 140.64 14.48 4 -2 0 76.04 15.85 4 -2 0 142.37 13.75 4 -2 0 119.96 12.18 4 -2 0 77.02 16.62 -4 2 0 111.19 12.82 -4 2 0 146.37 17.80 -4 2 0 106.11 17.69 -4 2 0 110.05 13.41 3 -2 0 553.78 37.53 3 -2 0 438.51 40.87 3 -2 0 502.46 37.57 3 -2 0 491.01 39.96 -3 2 0 495.65 40.07 -3 2 0 492.16 37.75 -3 2 0 432.15 40.38 -3 2 0 481.33 37.48 2 -2 0 199.02 15.26 2 -2 0 171.40 17.28 2 -2 0 186.67 15.05 2 -2 0 170.16 17.11 -2 2 0 176.97 16.94 -2 2 0 161.04 15.02 -2 2 0 174.28 15.47 -2 2 0 188.49 18.09 1 -2 0 668.82 46.61 1 -2 0 647.77 46.35 1 -2 0 566.49 47.44 1 -2 0 640.29 47.08 -1 2 0 639.37 47.61 -1 2 0 615.71 46.27 -1 2 0 646.54 47.12 -1 2 0 601.98 46.34 0 -2 0 1231.31 100.23 0 -2 0 1316.33 100.05 0 -2 0 1413.88 100.29 0 2 0 1321.55 100.05 0 2 0 1417.36 99.88 0 2 0 1418.17 100.35 0 2 0 1538.87 100.54 -1 -2 0 8.57 5.24 -1 -2 0 6.07 3.27 -1 -2 0 8.77 3.45 -1 -2 0 5.84 2.60 -1 -2 0 6.33 3.63 1 2 0 6.16 2.61 1 2 0 5.32 3.84 1 2 0 12.54 3.70 1 2 0 13.16 3.57 -2 -2 0 373.32 26.85 -2 -2 0 360.72 26.82 -2 -2 0 371.61 27.03 -2 -2 0 353.63 26.70 2 2 0 357.23 26.74 2 2 0 350.85 26.98 2 2 0 350.02 26.91 -3 -2 0 7081.80 522.76 -4 -2 0 516.08 41.12 -4 -2 0 597.36 41.60 -4 -2 0 589.65 40.65 -4 -2 0 531.67 40.82 -4 -2 0 536.61 41.20 4 2 0 550.86 41.32 4 2 0 555.72 41.22 4 2 0 527.17 41.37 4 2 0 569.36 42.23 4 2 0 516.09 41.89 4 2 0 564.96 40.44 -5 -2 0 43.50 7.43 -5 -2 0 41.89 9.09 -5 -2 0 53.00 9.84 -5 -2 0 42.83 8.70 -5 -2 0 51.04 6.50 5 2 0 44.64 10.18 5 2 0 42.37 8.97 5 2 0 46.25 11.75 5 2 0 32.96 10.41 5 2 0 31.75 8.54 -6 -2 0 136.76 15.71 -6 -2 0 150.26 14.24 -6 -2 0 151.57 16.91 -6 -2 0 147.99 13.50 6 2 0 153.06 16.41 6 2 0 109.73 17.55 6 2 0 152.29 16.09 6 2 0 125.49 17.70 6 2 0 154.56 17.25 -7 -2 0 296.85 24.29 -7 -2 0 227.75 23.70 -7 -2 0 241.43 20.67 -7 -2 0 242.89 21.80 -7 -2 0 293.09 25.41 7 2 0 220.60 25.86 7 2 0 221.21 26.14 7 2 0 247.25 23.72 7 2 0 225.08 23.57 -8 -2 0 112.29 17.59 -8 -2 0 69.76 16.50 8 2 0 78.62 18.06 8 2 0 97.88 20.22 -9 -2 0 23.21 16.57 9 2 0 12.59 20.44 9 2 0 49.56 19.01 -10 -2 0 53.69 18.38 10 2 0 65.68 22.22 10 2 0 10.37 23.48 9 -3 0 -14.18 21.70 -9 3 0 59.58 27.19 -9 3 0 29.97 29.97 8 -3 0 128.50 22.36 -8 3 0 116.89 27.86 -8 3 0 121.84 29.86 7 -3 0 249.40 25.45 7 -3 0 263.04 25.88 7 -3 0 250.19 28.60 -7 3 0 235.57 33.02 -7 3 0 222.80 31.58 6 -3 0 36.11 12.65 6 -3 0 67.89 14.67 6 -3 0 30.76 16.85 -6 3 0 50.20 22.54 -6 3 0 33.00 20.90 -6 3 0 -0.55 13.63 -6 3 0 35.02 13.37 5 -3 0 65.52 17.87 5 -3 0 75.20 12.66 5 -3 0 52.90 15.45 5 -3 0 94.60 13.08 5 -3 0 92.96 16.43 -5 3 0 66.89 20.28 -5 3 0 82.15 14.06 -5 3 0 67.88 14.09 -5 3 0 75.82 20.93 4 -3 0 481.34 39.93 4 -3 0 574.83 38.62 4 -3 0 404.55 43.11 4 -3 0 389.27 42.00 -4 3 0 513.79 39.08 -4 3 0 490.03 43.16 -4 3 0 506.14 43.97 -4 3 0 460.58 38.94 3 -3 0 771.44 55.55 3 -3 0 778.77 54.79 3 -3 0 776.42 57.60 3 -3 0 596.78 57.84 -3 3 0 713.95 54.55 -3 3 0 714.88 58.18 -3 3 0 685.76 54.68 -3 3 0 773.55 57.95 2 -3 0 3185.21 216.79 2 -3 0 3161.32 215.59 2 -3 0 3141.78 215.49 2 -3 0 2678.42 216.71 -2 3 0 2940.68 215.41 -2 3 0 2664.21 215.32 -2 3 0 3033.98 216.94 -2 3 0 2992.02 216.67 1 -3 0 401.03 33.40 1 -3 0 416.69 31.39 1 -3 0 428.98 32.55 1 -3 0 442.28 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107.23 13.69 -1 -2 -12 76.59 12.75 -1 -2 -12 68.99 15.08 1 2 12 98.64 13.93 1 2 12 93.90 16.96 1 2 12 80.41 18.96 -2 -2 -12 2021.88 152.96 -2 -2 -12 1875.05 155.35 -2 -2 -12 2267.97 152.26 2 2 12 2015.37 155.78 2 2 12 2171.56 154.45 2 2 12 2128.56 153.07 -3 -2 -12 113.91 25.68 -3 -2 -12 140.10 13.75 -3 -2 -12 88.59 16.89 3 2 12 156.66 22.57 3 2 12 104.18 17.30 3 2 12 131.61 23.26 -4 -2 -12 66.15 10.61 -4 -2 -12 68.93 21.10 4 2 12 62.30 21.76 4 2 12 56.00 17.01 4 2 12 50.03 22.58 -5 -2 -12 282.67 37.22 -5 -2 -12 250.56 22.51 5 2 12 257.93 29.36 -6 -2 -12 31.58 28.45 6 2 12 33.19 20.31 -7 -2 -12 102.31 32.89 7 2 12 131.68 31.98 -8 -2 -12 37.58 31.24 8 2 12 10.47 30.50 -9 -2 -12 100.49 32.20 9 2 12 55.53 34.58 6 -3 -12 13.71 21.36 -6 3 12 -15.17 31.37 5 -3 -12 62.58 20.16 -5 3 12 46.42 20.76 -5 3 12 32.05 30.99 4 -3 -12 37.73 17.26 -4 3 12 -17.40 19.14 -4 3 12 26.18 31.01 3 -3 -12 19.14 14.31 -3 3 12 -11.40 27.62 2 -3 -12 13.81 12.48 -2 3 12 8.16 25.91 -2 3 12 44.88 16.00 1 -3 -12 453.62 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-16 75.29 20.99 1 2 -16 19.19 20.27 -1 -2 16 7.02 19.79 0 2 -16 1.94 18.91 0 -2 16 -19.17 21.28 0 -2 16 -12.71 23.67 -1 2 -16 12.73 20.37 1 -2 16 16.97 22.92 1 -2 16 55.48 25.43 -2 2 -16 35.19 20.37 2 -2 16 -39.27 24.55 2 -2 16 30.65 24.83 -3 2 -16 26.41 19.87 3 -2 16 20.79 27.59 3 -2 16 8.75 24.68 3 1 -16 8.26 13.97 -3 -1 16 -54.99 34.63 2 1 -16 -1.37 17.23 1 1 -16 28.87 18.53 -1 -1 16 11.16 18.37 0 1 -16 -47.76 16.58 0 -1 16 -17.78 20.79 0 -1 16 -6.73 20.54 -1 1 -16 -13.37 17.63 1 -1 16 19.19 20.36 1 -1 16 8.86 21.05 -2 1 -16 43.36 18.13 2 -1 16 45.91 25.00 2 -1 16 23.75 22.10 -3 1 -16 -2.05 19.00 3 -1 16 -9.23 22.84 3 -1 16 -8.05 26.25 -4 1 -16 57.08 19.76 4 -1 16 18.38 25.49 4 -1 16 38.89 29.58 4 0 -16 10.18 18.73 -4 0 16 -33.12 35.22 3 0 -16 -16.56 16.77 -3 0 16 -32.06 33.93 2 0 -16 -10.14 17.72 -2 0 16 -5.71 16.81 1 0 -16 17.57 16.51 -1 0 16 12.02 18.59 0 0 -16 9.74 16.75 0 0 16 1.43 20.27 -1 0 -16 55.21 16.81 1 0 16 29.78 20.71 1 0 16 26.69 17.90 -2 0 -16 6.53 16.01 2 0 16 -21.49 21.86 2 0 16 3.57 20.90 -3 0 -16 25.29 15.90 3 0 16 35.72 25.98 3 0 16 32.82 21.49 -4 0 -16 1.49 14.99 4 0 16 4.26 22.46 4 0 16 -46.29 27.39 -5 0 -16 172.75 35.23 5 0 16 117.78 27.87 5 0 16 135.22 33.79 -4 1 16 57.64 38.30 -3 1 16 -22.34 35.12 2 -1 -16 -3.42 17.06 -2 1 16 15.94 17.35 -2 1 16 1.28 33.40 1 -1 -16 164.51 21.19 -1 1 16 108.10 23.18 0 -1 -16 10.58 16.10 0 1 16 -16.20 20.68 -1 -1 -16 -0.95 16.39 1 1 16 -30.88 18.51 1 1 16 -26.24 16.63 -2 -1 -16 47.59 16.11 2 1 16 104.22 19.36 2 1 16 54.97 23.20 -3 -1 -16 43.79 15.97 3 1 16 27.67 19.59 3 1 16 -22.91 23.94 -4 -1 -16 32.53 31.13 4 1 16 -13.46 20.62 4 1 16 -45.47 26.29 -5 -1 -16 29.26 25.73 5 1 16 13.14 29.93 5 1 16 24.50 23.12 -6 -1 -16 79.52 36.98 6 1 16 36.12 24.05 6 1 16 17.40 32.84 4 -2 -16 46.00 23.06 -4 2 16 63.65 37.54 -3 2 16 -15.40 36.13 -2 2 16 9.41 34.69 -2 2 16 -4.31 19.34 -1 2 16 12.47 20.13 -1 2 16 45.70 32.54 0 -2 -16 144.62 19.81 0 2 16 133.70 24.65 -1 -2 -16 96.43 17.54 1 2 16 112.39 22.79 -2 -2 -16 7.66 15.25 2 2 16 -6.29 17.44 2 2 16 1.81 21.57 -3 -2 -16 72.12 29.55 -3 -2 -16 104.79 17.24 3 2 16 94.26 26.39 3 2 16 96.09 20.38 -4 -2 -16 7.18 30.19 4 2 16 -29.26 24.95 -5 -2 -16 88.47 34.97 5 2 16 35.46 31.09 -6 -2 -16 82.55 36.87 6 2 16 -24.33 31.58 4 -3 -16 12.85 22.26 -4 3 16 81.00 38.81 3 -3 -16 3.44 19.90 -3 3 16 -5.73 36.14 2 -3 -16 -7.19 18.94 -2 3 16 -7.43 33.55 -2 3 16 1.65 19.87 -1 3 16 -5.81 21.32 -1 3 16 24.83 33.66 0 3 16 262.22 42.81 0 3 16 308.15 32.14 1 3 16 -10.97 19.90 2 3 16 107.97 24.88 -3 -3 -16 -5.29 11.34 -3 -3 -16 42.17 26.55 3 3 16 0.81 23.46 -4 -3 -16 108.93 32.49 4 3 16 73.26 27.61 -5 -3 -16 25.61 24.48 5 3 16 3.35 28.39 -6 -3 -16 27.91 33.92 6 3 16 39.13 33.44 3 -4 -16 -27.36 19.57 -3 4 16 -18.32 26.55 -3 4 16 -34.80 36.38 2 -4 -16 13.98 17.86 -2 4 16 0.06 36.30 -2 4 16 36.24 20.75 1 -4 -16 74.83 18.83 -1 4 16 64.73 36.51 -1 4 16 48.36 21.71 0 4 16 155.91 25.37 0 4 16 111.05 36.36 1 4 16 78.40 33.56 1 4 16 55.31 22.27 -2 -4 -16 -26.31 21.72 2 4 16 -13.14 22.16 -3 -4 -16 165.29 26.73 3 4 16 163.61 28.99 -4 -4 -16 3.23 29.35 4 4 16 20.46 27.00 -5 -4 -16 19.18 31.86 5 4 16 -21.29 28.87 -6 -4 -16 34.34 34.77 6 4 16 35.30 25.02 -7 -4 -16 -32.48 33.68 7 4 16 0.50 34.74 3 -5 -16 -22.20 20.47 -3 5 16 -6.41 27.06 -3 5 16 -14.50 37.02 2 -5 -16 -11.25 18.65 -2 5 16 -29.61 35.46 -1 5 16 8.94 35.39 -1 5 16 1.23 24.43 0 5 16 66.38 26.08 0 5 16 91.80 36.81 1 5 16 111.92 37.15 1 5 16 108.08 25.23 -2 -5 -16 13.79 23.13 2 5 16 12.38 33.88 2 5 16 15.95 23.64 -3 -5 -16 -4.54 24.65 3 5 16 16.91 24.89 3 5 16 1.81 32.50 -4 -5 -16 95.95 30.89 4 5 16 57.86 28.85 -5 -5 -16 28.33 31.92 5 5 16 -11.74 29.31 -6 -5 -16 35.25 33.83 6 5 16 -14.06 32.63 2 -6 -16 45.75 20.99 -2 6 16 103.07 39.87 -1 6 16 -14.08 34.74 -1 6 16 42.44 26.49 0 6 16 39.13 24.74 0 6 16 110.17 39.08 1 6 16 164.67 40.34 1 6 16 161.30 28.96 -2 -6 -16 -8.02 23.21 2 6 16 -9.93 33.53 2 6 16 38.10 24.93 -3 -6 -16 162.26 30.91 3 6 16 132.33 30.25 3 6 16 124.74 37.30 -4 -6 -16 -10.58 28.12 4 6 16 -44.25 32.46 4 6 16 -6.89 28.11 -5 -6 -16 112.51 33.69 5 6 16 80.83 32.38 -6 -6 -16 56.46 33.24 6 6 16 32.30 34.03 -1 7 16 75.15 38.66 0 7 16 44.50 37.44 0 7 16 34.72 26.31 1 7 16 108.70 28.19 1 7 16 34.98 35.88 -2 -7 -16 73.14 26.58 2 7 16 67.55 27.90 2 7 16 50.31 39.42 -3 -7 -16 -33.04 26.51 3 7 16 -29.04 36.98 3 7 16 33.74 27.12 -4 -7 -16 248.02 37.05 4 7 16 198.72 36.55 -5 -7 -16 -41.25 30.53 5 7 16 -1.61 24.05 1 8 16 57.22 28.64 1 8 16 28.19 40.54 -2 -8 -16 101.41 29.22 2 8 16 69.20 40.13 2 8 16 50.30 29.28 -3 -8 -16 94.94 30.22 3 8 16 102.78 32.02 -4 -8 -16 5.36 30.68 4 8 16 5.35 30.46 2 1 -17 27.61 19.33 1 1 -17 24.34 19.86 -1 -1 17 12.01 20.85 0 1 -17 61.36 20.69 0 -1 17 54.39 23.30 -1 1 -17 -12.08 17.94 1 -1 17 -51.62 23.03 1 -1 17 -48.44 21.41 -2 1 -17 40.89 19.15 2 -1 17 -10.23 23.12 2 -1 17 -10.12 25.02 -3 1 -17 -8.09 17.93 3 -1 17 -30.31 30.67 3 -1 17 -0.89 24.70 2 0 -17 34.22 19.22 1 0 -17 -5.71 17.75 -1 0 17 -4.45 20.29 0 0 -17 22.50 18.54 0 0 17 -16.22 19.25 -1 0 -17 29.71 17.92 1 0 17 89.22 25.92 -2 0 -17 30.54 17.03 2 0 17 25.25 24.45 2 0 17 20.17 22.67 -3 0 -17 -9.37 18.17 3 0 17 -12.31 21.99 3 0 17 -14.23 25.78 4 0 17 -33.21 27.90 4 0 17 -20.61 23.08 -3 1 17 -10.24 36.78 2 -1 -17 43.49 19.38 -2 1 17 67.88 37.98 -2 1 17 48.02 19.40 1 -1 -17 114.77 21.11 -1 1 17 110.63 23.42 0 -1 -17 37.35 17.62 0 1 17 35.85 22.78 -1 -1 -17 35.27 16.28 1 1 17 22.69 21.68 -2 -1 -17 43.05 17.96 2 1 17 8.86 18.16 2 1 17 18.17 26.29 -3 -1 -17 4.23 15.04 3 1 17 -10.78 25.17 3 1 17 -7.11 19.97 4 1 17 -28.56 21.09 4 1 17 -10.34 22.06 5 1 17 32.18 26.60 5 1 17 72.26 32.98 -3 2 17 -27.37 37.61 -2 2 17 -44.36 34.32 -2 2 17 7.36 19.92 -1 2 17 74.90 23.37 -1 2 17 99.18 37.25 0 -2 -17 -26.36 16.69 0 2 17 14.48 22.74 -1 -2 -17 111.89 18.88 1 2 17 93.33 23.88 -2 -2 -17 13.49 16.41 2 2 17 -14.93 22.69 -3 -2 -17 23.10 15.96 3 2 17 38.78 26.01 4 2 17 92.68 29.90 -5 -2 -17 13.63 33.61 5 2 17 -46.82 29.89 -3 3 17 -29.80 38.17 -2 3 17 75.24 37.56 -2 3 17 53.95 23.20 -1 3 17 8.83 28.07 -1 3 17 -3.40 19.97 0 3 17 68.19 24.84 0 3 17 53.97 35.11 1 3 17 -6.22 21.19 2 3 17 150.13 27.63 3 3 17 0.53 24.50 -4 -3 -17 -0.92 30.75 4 3 17 -3.90 26.79 -5 -3 -17 144.84 36.66 5 3 17 119.33 33.22 -6 -3 -17 65.06 36.87 6 3 17 91.89 35.81 -2 4 17 29.55 39.08 -2 4 17 20.16 23.77 -1 4 17 44.74 37.64 -1 4 17 85.27 26.05 0 4 17 -58.68 34.29 0 4 17 14.61 21.87 1 4 17 14.50 35.22 1 4 17 11.56 24.92 2 4 17 -6.26 22.64 3 4 17 132.12 27.99 -4 -4 -17 75.92 31.53 4 4 17 47.14 28.75 -5 -4 -17 -5.57 33.39 5 4 17 -59.14 29.74 -6 -4 -17 24.31 34.43 6 4 17 61.23 34.29 2 -5 -17 7.61 22.01 -2 5 17 -5.59 39.27 -1 5 17 54.94 31.31 -1 5 17 34.84 26.21 0 5 17 127.95 40.01 0 5 17 120.33 26.12 1 5 17 28.36 23.52 1 5 17 46.59 37.19 2 5 17 74.27 25.23 2 5 17 98.47 39.49 -3 -5 -17 15.92 27.33 3 5 17 17.35 26.55 3 5 17 -15.16 35.02 -4 -5 -17 43.50 30.15 4 5 17 21.66 21.90 -5 -5 -17 51.24 32.88 5 5 17 -42.05 29.12 -1 6 17 40.29 28.61 -1 6 17 46.74 40.34 0 6 17 29.81 37.48 0 6 17 58.03 25.93 1 6 17 47.64 25.48 1 6 17 22.80 39.28 2 6 17 -60.90 40.42 2 6 17 9.79 25.62 -3 -6 -17 189.90 34.14 3 6 17 198.84 43.12 3 6 17 207.25 34.25 -4 -6 -17 -3.73 22.69 4 6 17 -35.40 28.61 4 6 17 -3.15 36.85 -5 -6 -17 69.31 27.02 5 6 17 55.23 33.35 1 7 17 5.86 38.05 1 7 17 16.02 26.56 2 7 17 38.41 27.68 2 7 17 0.82 38.42 -3 -7 -17 -12.08 27.82 3 7 17 19.63 27.79 3 7 17 -11.82 37.26 -4 -7 -17 52.52 30.88 4 7 17 12.72 30.40 0 0 -18 -0.78 19.02 0 0 18 0.87 23.57 -1 0 -18 15.67 18.93 1 0 18 -23.43 22.34 -2 0 -18 -8.57 18.26 2 0 18 -30.36 27.37 1 -1 -18 40.96 19.78 -1 1 18 13.62 22.56 0 -1 -18 44.50 19.22 0 1 18 70.62 22.06 -1 -1 -18 -5.85 17.11 1 1 18 -67.60 24.89 -2 -1 -18 14.92 17.21 2 1 18 35.41 25.22 -3 -1 -18 25.20 26.55 3 1 18 38.27 27.88 3 1 18 46.85 22.02 -1 2 18 16.75 36.84 -1 2 18 22.96 23.35 0 -2 -18 9.81 17.90 0 2 18 5.38 23.98 -1 -2 -18 21.69 17.59 1 2 18 41.34 23.30 -2 -2 -18 -0.30 15.91 2 2 18 -42.26 23.76 3 2 18 26.23 26.60 4 2 18 30.53 30.27 -1 3 18 43.83 24.84 -1 3 18 22.65 38.08 0 3 18 9.63 22.26 0 3 18 -51.69 35.13 1 3 18 -56.81 25.09 2 3 18 63.40 25.77 3 3 18 -8.23 25.81 4 3 18 -22.14 28.28 -1 4 18 64.79 23.94 -1 4 18 37.97 40.42 0 4 18 -84.42 37.05 0 4 18 5.77 25.56 1 4 18 78.91 39.51 1 4 18 51.94 25.04 2 4 18 -41.92 35.30 2 4 18 5.41 24.71 3 4 18 19.34 26.77 4 4 18 14.82 28.53 0 5 18 128.54 27.73 0 5 18 112.45 41.38 1 5 18 -3.20 23.50 1 5 18 8.08 38.38 2 5 18 270.50 35.17 2 5 18 219.96 46.69 3 5 18 -41.16 26.37 3 5 18 -30.59 38.88 4 5 18 49.46 31.01 1 6 18 -10.79 39.57 1 6 18 23.56 26.50 2 6 18 23.69 44.33 2 6 18 -2.66 19.47 3 6 18 58.10 28.68 3 6 18 18.47 40.23 0 0 0 0.00 0.00 _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 0.7454 _exptl_absorpt_correction_T_min 0.5312 _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 0.71096 8.762 8.909 15.129 73.592 82.034 75.610 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 9233 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.71946(7) 0.25497(6) 0.45846(3) 0.0817(2) Uani 1 1 d . . . . . Br2 Br 0.04723(6) 1.15148(6) 0.67133(4) 0.0845(2) Uani 1 1 d . . . . . O1 O 0.6974(3) 0.5786(3) 0.82034(15) 0.0430(6) Uani 1 1 d . . . . . O2 O 0.7510(3) 0.4296(3) 1.00258(18) 0.0544(7) Uani 1 1 d . . . . . H2O H 0.662(5) 0.469(6) 0.996(3) 0.082 Uiso 1 1 d . U . . . N1 N 0.5304(4) 0.3214(4) 0.9491(2) 0.0524(8) Uani 1 1 d . . . . . C1 C 0.6904(4) 0.6727(4) 0.7272(2) 0.0406(8) Uani 1 1 d . . . . . H1 H 0.778832 0.726955 0.711243 0.049 Uiso 1 1 calc R U . . . C2 C 0.5370(4) 0.7974(4) 0.7202(2) 0.0387(8) Uani 1 1 d . . . . . C3 C 0.4086(4) 0.7767(4) 0.7832(3) 0.0490(9) Uani 1 1 d . . . . . H3 H 0.419680 0.690080 0.835185 0.059 Uiso 1 1 calc R U . . . C4 C 0.2648(5) 0.8828(5) 0.7699(3) 0.0538(10) Uani 1 1 d . . . . . H4 H 0.178821 0.867418 0.812376 0.065 Uiso 1 1 calc R U . . . C5 C 0.2488(4) 1.0118(4) 0.6936(3) 0.0502(10) Uani 1 1 d . . . . . C6 C 0.3756(5) 1.0383(4) 0.6317(3) 0.0500(9) Uani 1 1 d . . . . . H6 H 0.364986 1.127522 0.581176 0.060 Uiso 1 1 calc R U . . . C7 C 0.5185(4) 0.9314(4) 0.6455(2) 0.0465(9) Uani 1 1 d . . . . . H7 H 0.604838 0.949228 0.603862 0.056 Uiso 1 1 calc R U . . . C8 C 0.6993(4) 0.5715(4) 0.6602(2) 0.0384(8) Uani 1 1 d . . . . . C9 C 0.7886(4) 0.5947(4) 0.5770(2) 0.0471(9) Uani 1 1 d . . . . . H9 H 0.847639 0.673165 0.561720 0.057 Uiso 1 1 calc R U . . . C10 C 0.7923(4) 0.5045(5) 0.5160(3) 0.0507(10) Uani 1 1 d . . . . . H10 H 0.851379 0.523596 0.459545 0.061 Uiso 1 1 calc R U . . . C11 C 0.7083(5) 0.3860(4) 0.5392(3) 0.0495(10) Uani 1 1 d . . . . . C12 C 0.6174(5) 0.3601(5) 0.6215(3) 0.0540(10) Uani 1 1 d . . . . . H12 H 0.560155 0.280105 0.637033 0.065 Uiso 1 1 calc R U . . . C13 C 0.6124(4) 0.4540(4) 0.6807(3) 0.0488(9) Uani 1 1 d . . . . . H13 H 0.549077 0.438218 0.735800 0.059 Uiso 1 1 calc R U . . . C14 C 0.8408(4) 0.4613(4) 0.8404(2) 0.0434(9) Uani 1 1 d . . . . . H14 H 0.866681 0.402262 0.792556 0.052 Uiso 1 1 calc R U . . . C15 C 0.9742(5) 0.5373(5) 0.8404(3) 0.0626(11) Uani 1 1 d . . . . . H15 H 0.966156 0.597729 0.882638 0.075 Uiso 1 1 calc R U . . . C16 C 1.1002(6) 0.5240(6) 0.7852(4) 0.0883(16) Uani 1 1 d . . . . . H16A H 1.111382 0.464356 0.742249 0.106 Uiso 1 1 calc R U . . . H16B H 1.179886 0.574185 0.788297 0.106 Uiso 1 1 calc R U . . . C17 C 0.8045(4) 0.3444(4) 0.9334(2) 0.0453(9) Uani 1 1 d . . . . . C18 C 0.9552(5) 0.2241(5) 0.9665(3) 0.0628(11) Uani 1 1 d . . . . . H18A H 1.007160 0.175977 0.917767 0.094 Uiso 1 1 calc R U . . . H18B H 0.929247 0.142303 1.019122 0.094 Uiso 1 1 calc R U . . . H18C H 1.024282 0.278198 0.983445 0.094 Uiso 1 1 calc R U . . . C19 C 0.6788(5) 0.2627(4) 0.9206(2) 0.0461(9) Uani 1 1 d . . . . . C20 C 0.7158(5) 0.1372(5) 0.8787(3) 0.0604(11) Uani 1 1 d . . . . . H20 H 0.820295 0.096326 0.860682 0.073 Uiso 1 1 calc R U . . . C21 C 0.5961(7) 0.0733(5) 0.8639(3) 0.0737(13) Uani 1 1 d . . . . . H21 H 0.618776 -0.010551 0.835499 0.088 Uiso 1 1 calc R U . . . C22 C 0.4449(7) 0.1348(6) 0.8915(3) 0.0786(14) Uani 1 1 d . . . . . H22 H 0.361977 0.094798 0.881778 0.094 Uiso 1 1 calc R U . . . C23 C 0.4173(5) 0.2565(5) 0.9336(3) 0.0685(12) Uani 1 1 d . . . . . H23 H 0.313411 0.297006 0.952917 0.082 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 0.1212(5) 0.0737(3) 0.0609(3) -0.0330(2) -0.0165(3) -0.0175(3) Br2 0.0681(3) 0.0704(3) 0.0889(4) -0.0099(3) -0.0055(3) 0.0199(2) O1 0.0469(14) 0.0401(13) 0.0392(13) -0.0064(11) -0.0149(11) -0.0026(11) O2 0.0523(16) 0.0689(18) 0.0442(15) -0.0245(14) -0.0146(13) -0.0004(14) N1 0.0468(19) 0.0513(19) 0.058(2) -0.0146(16) -0.0064(16) -0.0077(16) C1 0.044(2) 0.0390(19) 0.040(2) -0.0079(16) -0.0078(16) -0.0103(16) C2 0.048(2) 0.0316(18) 0.0400(19) -0.0102(16) -0.0084(17) -0.0104(15) C3 0.057(2) 0.043(2) 0.041(2) -0.0025(17) -0.0043(19) -0.0080(18) C4 0.051(2) 0.054(2) 0.051(2) -0.013(2) 0.0037(19) -0.0067(19) C5 0.058(2) 0.041(2) 0.049(2) -0.0148(19) -0.006(2) 0.0007(18) C6 0.064(3) 0.035(2) 0.043(2) -0.0016(17) -0.009(2) -0.0038(18) C7 0.055(2) 0.039(2) 0.044(2) -0.0049(17) -0.0033(18) -0.0123(17) C8 0.0363(18) 0.039(2) 0.0366(19) -0.0045(16) -0.0112(16) -0.0049(15) C9 0.047(2) 0.041(2) 0.049(2) -0.0057(18) -0.0067(18) -0.0068(17) C10 0.055(2) 0.054(2) 0.039(2) -0.0134(19) 0.0010(18) -0.005(2) C11 0.060(2) 0.047(2) 0.042(2) -0.0139(18) -0.0196(19) -0.0008(19) C12 0.064(3) 0.053(2) 0.051(2) -0.013(2) -0.012(2) -0.021(2) C13 0.054(2) 0.055(2) 0.041(2) -0.0132(18) -0.0033(18) -0.0185(19) C14 0.041(2) 0.044(2) 0.048(2) -0.0140(17) -0.0170(17) -0.0043(16) C15 0.059(3) 0.067(3) 0.070(3) -0.018(2) -0.021(2) -0.019(2) C16 0.067(3) 0.099(4) 0.104(4) -0.009(3) -0.016(3) -0.041(3) C17 0.049(2) 0.046(2) 0.040(2) -0.0131(17) -0.0110(17) -0.0007(17) C18 0.057(2) 0.061(3) 0.060(3) -0.009(2) -0.019(2) 0.007(2) C19 0.057(2) 0.040(2) 0.036(2) -0.0034(16) -0.0083(17) -0.0068(18) C20 0.072(3) 0.054(3) 0.057(3) -0.020(2) 0.002(2) -0.013(2) C21 0.107(4) 0.059(3) 0.069(3) -0.029(2) 0.000(3) -0.032(3) C22 0.086(4) 0.075(3) 0.087(4) -0.022(3) -0.011(3) -0.036(3) C23 0.060(3) 0.065(3) 0.081(3) -0.015(3) -0.004(2) -0.019(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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C14 115.2(3) . . ? C17 O2 H2O 107(4) . . ? C19 N1 C23 117.3(4) . . ? O1 C1 C2 108.0(3) . . ? O1 C1 C8 112.0(3) . . ? C2 C1 C8 109.8(3) . . ? O1 C1 H1 109.0 . . ? C2 C1 H1 109.0 . . ? C8 C1 H1 109.0 . . ? C3 C2 C7 118.2(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 119.9(3) . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 120.8(3) . . ? C6 C5 Br2 119.5(3) . . ? C4 C5 Br2 119.7(3) . . ? C5 C6 C7 119.0(3) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C2 121.5(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? C9 C8 C13 117.8(3) . . ? C9 C8 C1 122.2(3) . . ? C13 C8 C1 120.0(3) . . ? C10 C9 C8 121.5(4) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 Br1 120.0(3) . . ? C12 C11 Br1 119.5(3) . . ? C11 C12 C13 119.2(4) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C8 121.5(3) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O1 C14 C15 111.4(3) . . ? O1 C14 C17 105.8(3) . . ? C15 C14 C17 114.0(3) . . ? O1 C14 H14 108.5 . . ? C15 C14 H14 108.5 . . ? C17 C14 H14 108.5 . . ? C16 C15 C14 123.7(4) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C15 C16 H16A 120.0 . . ? C15 C16 H16B 120.0 . . ? H16A C16 H16B 120.0 . . ? O2 C17 C19 110.7(3) . . ? O2 C17 C18 105.6(3) . . ? C19 C17 C18 112.1(3) . . ? O2 C17 C14 110.0(3) . . ? C19 C17 C14 108.3(3) . . ? C18 C17 C14 110.1(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 C20 121.7(4) . . ? N1 C19 C17 116.7(3) . . ? C20 C19 C17 121.6(4) . . ? C21 C20 C19 119.4(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 118.9(4) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C21 C22 C23 118.6(4) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N1 C23 C22 124.1(4) . . ? N1 C23 H23 118.0 . . ? C22 C23 H23 118.0 . . ? 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 C11 1.891(4) . ? Br2 C5 1.901(4) . ? O1 C1 1.423(4) . ? O1 C14 1.426(4) . ? O2 C17 1.423(4) . ? O2 H2O 0.78(5) . ? N1 C19 1.334(5) . ? N1 C23 1.341(5) . ? C1 C2 1.510(5) . ? C1 C8 1.518(5) . ? C1 H1 0.9800 . ? C2 C3 1.383(5) . ? C2 C7 1.386(5) . ? C3 C4 1.375(5) . ? C3 H3 0.9300 . ? C4 C5 1.375(5) . ? C4 H4 0.9300 . ? C5 C6 1.372(5) . ? C6 C7 1.373(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.378(5) . ? C8 C13 1.385(5) . ? C9 C10 1.377(5) . ? C9 H9 0.9300 . ? C10 C11 1.373(5) . ? C10 H10 0.9300 . ? C11 C12 1.375(5) . ? C12 C13 1.378(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.489(5) . ? C14 C17 1.543(5) . ? C14 H14 0.9800 . ? C15 C16 1.290(6) . ? C15 H15 0.9300 . ? C16 H16A 0.9300 . ? C16 H16B 0.9300 . ? C17 C19 1.523(5) . ? C17 C18 1.523(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.385(5) . ? C20 C21 1.381(6) . ? C20 H20 0.9300 . ? C21 C22 1.357(7) . ? C21 H21 0.9300 . ? C22 C23 1.362(6) . ? C22 H22 0.9300 . ? C23 H23 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 C14 O1 C1 C2 -175.8(3) . . . . ? C14 O1 C1 C8 63.1(3) . . . . ? O1 C1 C2 C3 -22.7(4) . . . . ? C8 C1 C2 C3 99.7(4) . . . . ? O1 C1 C2 C7 162.1(3) . . . . ? C8 C1 C2 C7 -75.5(4) . . . . ? C7 C2 C3 C4 2.6(5) . . . . ? C1 C2 C3 C4 -172.7(3) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 -1.8(6) . . . . ? C3 C4 C5 Br2 176.4(3) . . . . ? C4 C5 C6 C7 2.0(6) . . . . ? Br2 C5 C6 C7 -176.2(3) . . . . ? C5 C6 C7 C2 0.2(6) . . . . ? C3 C2 C7 C6 -2.5(5) . . . . ? C1 C2 C7 C6 172.9(3) . . . . ? O1 C1 C8 C9 -138.1(3) . . . . ? C2 C1 C8 C9 101.9(4) . . . . ? O1 C1 C8 C13 43.7(4) . . . . ? C2 C1 C8 C13 -76.3(4) . . . . ? C13 C8 C9 C10 -0.2(5) . . . . ? C1 C8 C9 C10 -178.4(3) . . . . ? C8 C9 C10 C11 -1.5(5) . . . . ? C9 C10 C11 C12 1.8(5) . . . . ? C9 C10 C11 Br1 -177.3(3) . . . . ? C10 C11 C12 C13 -0.3(6) . . . . ? Br1 C11 C12 C13 178.8(3) . . . . ? C11 C12 C13 C8 -1.4(6) . . . . ? C9 C8 C13 C12 1.7(5) . . . . ? C1 C8 C13 C12 179.9(3) . . . . ? C1 O1 C14 C15 71.7(4) . . . . ? C1 O1 C14 C17 -163.8(3) . . . . ? O1 C14 C15 C16 -119.3(5) . . . . ? C17 C14 C15 C16 121.0(5) . . . . ? O1 C14 C17 O2 -57.9(3) . . . . ? C15 C14 C17 O2 64.9(4) . . . . ? O1 C14 C17 C19 63.2(3) . . . . ? C15 C14 C17 C19 -174.0(3) . . . . ? O1 C14 C17 C18 -173.9(3) . . . . ? C15 C14 C17 C18 -51.1(4) . . . . ? C23 N1 C19 C20 -1.5(5) . . . . ? C23 N1 C19 C17 176.4(3) . . . . ? O2 C17 C19 N1 21.2(4) . . . . ? C18 C17 C19 N1 138.8(3) . . . . ? C14 C17 C19 N1 -99.5(4) . . . . ? O2 C17 C19 C20 -160.9(3) . . . . ? C18 C17 C19 C20 -43.2(5) . . . . ? C14 C17 C19 C20 78.5(4) . . . . ? N1 C19 C20 C21 1.6(6) . . . . ? C17 C19 C20 C21 -176.3(4) . . . . ? C19 C20 C21 C22 -0.4(7) . . . . ? C20 C21 C22 C23 -0.7(7) . . . . ? C19 N1 C23 C22 0.4(6) . . . . ? C21 C22 C23 N1 0.7(7) . . . . ?