#------------------------------------------------------------------------------ #$Date: 2016-08-05 06:36:36 +0300 (Fri, 05 Aug 2016) $ #$Revision: 184954 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/32/1543269.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_1543269 loop_ _publ_author_name 'Xu, Ning' 'Gu, Da-Wei' 'Zi, Jing' 'Wu, Xin-Yan' 'Guo, Xun-Xiang' _publ_section_title ; Enantioselective Synthesis of 3-Alkynyl-3-hydroxyindolin-2-ones by Copper-Catalyzed Asymmetric Addition of Terminal Alkynes to Isatins. ; _journal_issue 10 _journal_name_full 'Organic letters' _journal_page_first 2439 _journal_page_last 2442 _journal_paper_doi 10.1021/acs.orglett.6b00971 _journal_volume 18 _journal_year 2016 _chemical_formula_moiety 'C23 H16 Br N O2' _chemical_formula_sum 'C23 H16 Br N O2' _chemical_formula_weight 418.28 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 116.7950(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 17.9232(8) _cell_length_b 12.4144(5) _cell_length_c 19.2095(8) _cell_measurement_reflns_used 9932 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 68.290 _cell_measurement_theta_min 4.30 _cell_volume 3815.3(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.968 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0226 _diffrn_reflns_Laue_measured_fraction_full 0.968 _diffrn_reflns_Laue_measured_fraction_max 0.968 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18484 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.290 _diffrn_reflns_theta_min 4.508 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.456 _exptl_crystal_description block _exptl_crystal_F_000 1696 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.507 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.256 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 3380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.256 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0360 _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^)+(0.0533P)^2^+10.1969P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1109 _refine_ls_wR_factor_ref 0.1215 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full 0.968 _reflns_Friedel_fraction_max 0.922 _reflns_number_gt 3241 _reflns_number_total 3380 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol6b00971_si_002.cif _cod_data_source_block p _cod_depositor_comments 'Adding full bibliography for 1543269.cif.' _cod_database_code 1543269 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL p in C2/c CELL 1.54178 17.9232 12.4144 19.2095 90.000 116.795 90.000 ZERR 8.00 0.0008 0.0005 0.0008 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O Br UNIT 184 128 8 16 8 L.S. 30 BOND ACTA FMAP 2 PLAN 20 HTAB O1 O2_$2 HTAB C17 Br1_$1 HTAB O1 O2_$2 EQIV $2 -x+1, -y+1, -z+1 HTAB C17 Br1_$1 EQIV $1 x+1/2, -y+1/2, z+1/2 Htab HTAB C17 Br1_$1 HTAB O1 O2_$2 HTAB C17 Br1_$1 HTAB O1 O2_$2 TEMP -93.150 WGHT 0.053300 10.196900 FVAR 0.12429 BR1 5 0.132271 0.104127 0.243814 11.00000 0.03110 0.03388 = 0.03092 -0.00905 0.00620 -0.00614 C1 1 0.214735 0.156725 0.340671 11.00000 0.02190 0.02066 = 0.02978 -0.00572 0.01185 -0.00057 C2 1 0.252221 0.256160 0.343146 11.00000 0.02294 0.01901 = 0.02540 -0.00054 0.01190 0.00272 AFIX 43 H2A 2 0.235892 0.299191 0.297710 11.00000 -1.20000 AFIX 0 C3 1 0.313724 0.289067 0.414111 11.00000 0.02249 0.01550 = 0.02717 -0.00100 0.01496 0.00079 C4 1 0.336650 0.226161 0.480819 11.00000 0.01908 0.01848 = 0.02482 -0.00218 0.01189 0.00201 C5 1 0.298241 0.128462 0.478553 11.00000 0.02421 0.01715 = 0.02905 0.00098 0.01419 -0.00091 AFIX 43 H5A 2 0.313617 0.086483 0.524337 11.00000 -1.20000 AFIX 0 C6 1 0.236339 0.094111 0.406770 11.00000 0.02423 0.01694 = 0.03750 -0.00341 0.01744 -0.00237 AFIX 43 H6A 2 0.208737 0.027455 0.403009 11.00000 -1.20000 AFIX 0 C7 1 0.366014 0.390929 0.437057 11.00000 0.02732 0.01952 = 0.02658 -0.00213 0.01503 -0.00406 C8 1 0.420724 0.373939 0.526493 11.00000 0.02584 0.02167 = 0.02726 -0.00262 0.01490 -0.00226 C9 1 0.313530 0.487987 0.422611 11.00000 0.03602 0.01918 = 0.02742 -0.00060 0.01681 -0.00364 C10 1 0.267074 0.563351 0.409075 11.00000 0.03822 0.02148 = 0.03348 -0.00021 0.01992 -0.00200 C11 1 0.210253 0.653606 0.390000 11.00000 0.03642 0.01819 = 0.03661 -0.00298 0.01668 0.00069 C12 1 0.193752 0.714767 0.324841 11.00000 0.05724 0.03500 = 0.04842 0.00869 0.03169 0.01295 AFIX 43 H12A 2 0.220071 0.697351 0.293032 11.00000 -1.20000 AFIX 0 C13 1 0.139222 0.801427 0.305078 11.00000 0.06835 0.03703 = 0.05894 0.01615 0.02640 0.01872 AFIX 43 H13A 2 0.128002 0.842446 0.259668 11.00000 -1.20000 AFIX 0 C14 1 0.101476 0.828065 0.350861 11.00000 0.03684 0.02946 = 0.06997 -0.00429 0.01231 0.00879 AFIX 43 H14A 2 0.064812 0.888155 0.337731 11.00000 -1.20000 AFIX 0 C15 1 0.116844 0.767531 0.415868 11.00000 0.06783 0.05111 = 0.08173 -0.00315 0.04755 0.01825 AFIX 43 H15A 2 0.090019 0.785310 0.447184 11.00000 -1.20000 AFIX 0 C16 1 0.171360 0.680510 0.436059 11.00000 0.07276 0.04386 = 0.05643 0.00813 0.04349 0.01731 AFIX 43 H16A 2 0.182082 0.639381 0.481306 11.00000 -1.20000 AFIX 0 C17 1 0.438695 0.230998 0.624085 11.00000 0.02221 0.02840 = 0.02281 -0.00015 0.01140 0.00233 AFIX 23 H17A 2 0.394848 0.206584 0.638408 11.00000 -1.20000 H17B 2 0.472236 0.287065 0.661918 11.00000 -1.20000 AFIX 0 C18 1 0.494469 0.137119 0.629654 11.00000 0.02754 0.03150 = 0.02656 0.00201 0.01302 0.00716 C19 1 0.561740 0.151661 0.613488 11.00000 0.05669 0.04493 = 0.08067 0.01148 0.05009 0.01498 AFIX 43 H19A 2 0.571872 0.220281 0.597552 11.00000 -1.20000 AFIX 0 C20 1 0.614250 0.065816 0.620624 11.00000 0.08896 0.06580 = 0.13926 0.02357 0.09248 0.03416 AFIX 43 H20A 2 0.661064 0.075854 0.610589 11.00000 -1.20000 AFIX 0 C21 1 0.598228 -0.034865 0.642475 11.00000 0.08419 0.05873 = 0.11436 0.02386 0.06616 0.04217 AFIX 43 H21A 2 0.632481 -0.094432 0.644635 11.00000 -1.20000 AFIX 0 C22 1 0.533812 -0.048854 0.660824 11.00000 0.05972 0.04099 = 0.08827 0.02677 0.03240 0.01960 AFIX 43 H22A 2 0.524331 -0.117234 0.677585 11.00000 -1.20000 AFIX 0 C23 1 0.481831 0.038006 0.654822 11.00000 0.03777 0.04055 = 0.05709 0.01938 0.02529 0.01272 AFIX 43 H23A 2 0.437283 0.028698 0.668226 11.00000 -1.20000 AFIX 0 N1 3 0.399055 0.277790 0.546017 11.00000 0.02079 0.01965 = 0.02320 -0.00123 0.00945 -0.00207 O1 4 0.418355 0.393524 0.399587 11.00000 0.03332 0.02659 = 0.03584 -0.00604 0.02305 -0.00849 AFIX 83 H1A 2 0.448035 0.449315 0.413127 11.00000 -1.50000 AFIX 0 O2 4 0.474628 0.434365 0.570475 11.00000 0.03375 0.03086 = 0.03154 -0.00629 0.01135 -0.01408 HKLF 4 REM p in C2/c REM R1 = 0.0360 for 3241 Fo > 4sig(Fo) and 0.0394 for all 3380 data REM 244 parameters refined using 0 restraints END WGHT 0.0533 10.1969 REM Instructions for potential hydrogen bonds HTAB C17 Br1_$1 HTAB O1 O2_$2 REM Highest difference peak 0.507, deepest hole -0.554, 1-sigma level 0.162 Q1 1 0.5449 -0.0775 0.6176 11.00000 0.05 0.51 Q2 1 0.5919 -0.1243 0.6067 11.00000 0.05 0.47 Q3 1 0.1174 0.1559 0.2098 11.00000 0.05 0.47 Q4 1 0.5049 0.3609 0.7260 11.00000 0.05 0.43 Q5 1 0.5206 0.3899 0.6993 11.00000 0.05 0.42 Q6 1 0.5586 0.0114 0.5741 11.00000 0.05 0.42 Q7 1 0.3986 0.1355 0.4781 11.00000 0.05 0.41 Q8 1 0.5283 -0.1167 0.7312 11.00000 0.05 0.41 Q9 1 0.3767 0.1340 0.5907 11.00000 0.05 0.40 Q10 1 0.1564 0.8261 0.3520 11.00000 0.05 0.40 Q11 1 0.5410 0.3939 0.6002 11.00000 0.05 0.39 Q12 1 0.3235 0.1774 0.4819 11.00000 0.05 0.39 Q13 1 0.5588 -0.1129 0.7082 11.00000 0.05 0.38 Q14 1 0.5782 -0.0495 0.6921 11.00000 0.05 0.38 Q15 1 0.2073 0.8807 0.3236 11.00000 0.05 0.37 Q16 1 0.5153 0.1102 0.5684 11.00000 0.05 0.37 Q17 1 0.5518 0.3530 0.6533 11.00000 0.05 0.37 Q18 1 0.4073 0.5936 0.4785 11.00000 0.05 0.36 Q19 1 0.2153 0.8293 0.3433 11.00000 0.05 0.36 Q20 1 0.3144 0.1382 0.6307 11.00000 0.05 0.36 ; _shelx_res_checksum 4961 _shelx_hkl_file ; -2 0 0 43.77 1.59 -2 0 0 44.41 1.59 2 0 0 43.72 1.60 -6 0 0 1.52 0.12 -8 0 0 303.64 10.96 14 0 0 34.07 1.86 16 0 0 69.75 3.15 18 0 0 61.59 2.92 -1 -1 0 174.02 6.31 1 1 0 174.68 6.31 5 -1 0 250.27 8.95 -5 -1 0 252.02 8.99 -5 1 0 242.82 8.96 -7 -1 0 100.95 3.70 -9 -1 0 46.60 1.69 -9 -1 0 42.92 1.74 -11 -1 0 190.14 7.05 -13 -1 0 2.52 0.48 13 1 0 1.74 0.45 13 1 0 2.69 0.41 -15 -1 0 35.95 1.48 15 -1 0 29.46 1.95 15 1 0 35.10 1.94 -17 -1 0 0.59 0.42 19 1 0 122.03 4.74 0 -2 0 99.97 3.72 0 2 0 102.88 3.72 2 -2 0 248.77 9.44 -2 -2 0 263.73 9.46 -2 -2 0 273.35 9.48 2 2 0 262.75 9.46 2 2 0 256.91 9.45 -4 -2 0 56.38 2.17 -4 2 0 54.71 2.11 4 2 0 56.89 2.14 4 2 0 60.75 2.13 -6 -2 0 31.05 1.18 6 2 0 29.23 1.12 -6 2 0 28.09 1.15 6 2 0 31.49 1.12 -8 -2 0 72.22 2.83 -8 -2 0 78.91 2.83 -10 -2 0 8.09 0.55 -10 -2 0 8.58 0.57 -12 -2 0 27.06 1.21 12 2 0 26.73 1.25 12 2 0 28.89 1.67 -14 -2 0 4.10 0.57 18 2 0 42.06 2.37 -1 -3 0 270.97 9.66 1 -3 0 264.57 9.65 -1 3 0 270.52 9.65 1 3 0 260.69 9.65 -3 -3 0 39.74 1.54 3 -3 0 41.16 1.52 5 -3 0 733.97 26.46 -7 -3 0 84.07 3.09 -7 -3 0 81.73 3.08 7 3 0 80.89 3.02 -9 -3 0 93.32 3.51 -11 -3 0 37.52 1.66 -11 -3 0 37.14 1.56 -13 -3 0 1.34 0.45 -13 -3 0 1.49 0.37 13 3 0 1.43 0.34 -15 -3 0 1.41 0.71 -15 -3 0 1.53 0.40 0 -4 0 603.29 21.80 2 -4 0 2.04 0.19 -2 -4 0 2.25 0.21 2 4 0 1.85 0.17 4 -4 0 227.63 8.06 -4 -4 0 214.99 8.10 4 4 0 222.55 8.08 -6 -4 0 4.52 0.35 -6 -4 0 4.27 0.38 6 4 0 3.93 0.33 -8 -4 0 245.12 9.05 -8 -4 0 249.36 9.08 -10 -4 0 6.62 0.55 -10 -4 0 6.88 0.63 -10 -4 0 7.02 0.72 -12 -4 0 113.95 4.26 -12 -4 0 107.92 4.27 12 4 0 113.23 4.57 12 4 0 112.28 4.25 -14 -4 0 194.77 7.50 -14 -4 0 197.49 7.50 14 4 0 203.38 7.48 14 4 0 212.53 7.82 -18 -4 0 23.54 1.08 1 -5 0 423.89 14.96 -1 -5 0 414.12 14.97 -1 5 0 409.66 14.95 1 5 0 402.17 14.95 -3 -5 0 164.54 6.09 3 -5 0 166.21 6.06 3 5 0 162.89 6.07 -3 5 0 167.29 6.06 -5 -5 0 169.83 6.24 -5 -5 0 167.19 6.20 -5 5 0 172.13 6.18 5 5 0 168.28 6.20 -5 5 0 164.92 6.16 -7 -5 0 140.11 5.21 -7 -5 0 143.30 5.25 -7 5 0 136.73 5.14 -9 -5 0 4.34 0.60 -9 -5 0 4.18 0.62 -9 -5 0 3.79 0.48 -11 -5 0 231.51 8.59 -11 -5 0 238.38 8.58 -11 -5 0 229.52 8.55 11 5 0 231.22 8.57 11 5 0 230.61 8.84 -13 -5 0 25.14 1.41 -13 -5 0 21.12 1.18 -13 -5 0 22.76 1.18 13 5 0 26.04 1.64 13 5 0 20.25 1.10 -15 -5 0 59.87 2.42 -15 -5 0 58.83 2.43 15 5 0 59.86 2.36 -17 -5 0 0.39 0.34 -17 -5 0 0.14 0.53 0 -6 0 520.63 18.83 0 6 0 516.86 18.80 0 6 0 519.73 18.82 -2 -6 0 4.11 0.37 2 -6 0 4.41 0.39 -2 6 0 3.40 0.36 2 6 0 3.64 0.34 2 6 0 3.66 0.51 -2 6 0 3.97 0.33 -4 -6 0 154.53 5.62 -4 -6 0 148.91 5.57 -4 6 0 149.41 5.57 -4 6 0 148.88 5.53 4 6 0 150.92 5.59 -6 -6 0 7.46 0.56 -6 -6 0 6.65 0.65 -6 -6 0 7.07 0.54 6 6 0 7.11 0.56 -6 6 0 6.65 0.53 -6 6 0 7.84 0.49 -8 -6 0 299.56 11.01 -8 -6 0 303.57 11.02 -8 -6 0 295.63 11.08 -8 6 0 303.33 10.94 -10 -6 0 110.95 4.17 -10 -6 0 111.07 4.16 -10 -6 0 106.54 4.11 -10 6 0 111.93 4.07 10 6 0 108.48 4.13 10 6 0 102.89 4.47 -12 -6 0 9.75 0.79 -12 -6 0 9.20 0.79 -12 6 0 9.65 0.69 -16 -6 0 19.75 1.08 -16 -6 0 20.63 1.05 1 -7 0 45.06 1.86 -1 7 0 46.67 1.82 1 7 0 44.16 1.83 -1 7 0 46.61 1.84 -3 -7 0 3.13 0.42 -3 -7 0 2.98 0.53 -3 7 0 2.28 0.36 -3 7 0 2.10 0.35 3 7 0 2.12 0.39 3 7 0 1.95 0.49 -5 -7 0 6.38 0.64 -5 -7 0 6.47 0.63 -5 7 0 5.65 0.44 5 7 0 6.25 0.54 -5 7 0 4.36 0.64 -7 -7 0 12.94 0.79 -7 -7 0 14.06 0.82 -7 -7 0 13.66 0.91 -7 7 0 13.51 0.70 -7 7 0 14.33 1.13 7 7 0 10.80 0.87 -9 -7 0 32.81 1.48 -9 -7 0 32.51 1.48 -9 -7 0 31.20 1.41 9 7 0 32.71 1.61 9 7 0 32.84 1.47 9 7 0 31.52 1.55 -9 7 0 34.11 1.38 -11 -7 0 8.11 0.78 -11 -7 0 7.89 0.76 -11 7 0 8.79 0.63 0 8 0 120.35 4.51 0 8 0 114.51 4.45 0 8 0 119.78 4.45 -2 -8 0 4.56 0.57 -2 8 0 4.56 0.45 2 8 0 3.80 0.53 2 8 0 3.75 0.66 2 8 0 4.26 0.61 -2 8 0 4.44 0.53 -2 8 0 5.03 0.53 -4 -8 0 78.35 3.35 -4 -8 0 84.00 3.29 -4 -8 0 86.76 3.40 -4 8 0 87.57 3.28 4 8 0 86.07 3.38 -4 8 0 85.42 3.34 -4 8 0 88.28 3.26 -6 -8 0 12.97 0.82 -6 -8 0 10.52 1.00 -6 -8 0 12.08 0.81 6 8 0 14.16 1.17 6 8 0 11.16 0.89 -6 8 0 11.02 0.79 -6 8 0 10.77 0.67 -8 -8 0 12.34 0.88 -8 -8 0 12.88 0.87 -8 -8 0 12.19 0.81 8 8 0 13.33 0.87 -8 8 0 12.82 0.88 8 8 0 12.42 0.92 8 8 0 13.85 1.04 -8 8 0 13.74 0.75 -10 -8 0 1.51 0.47 -10 -8 0 0.11 0.39 -10 8 0 0.33 0.43 10 8 0 1.04 0.48 -10 8 0 0.98 0.31 -12 -8 0 8.40 0.66 -12 -8 0 7.76 0.78 -12 -8 0 6.73 0.74 12 8 0 8.39 0.62 -12 8 0 7.10 0.64 -14 -8 0 22.88 1.14 -14 -8 0 22.55 1.20 -14 -8 0 23.32 1.07 14 8 0 23.04 1.07 14 8 0 24.71 1.59 -16 -8 0 33.08 1.36 -16 -8 0 35.21 1.43 -1 -9 0 219.48 8.29 1 9 0 217.20 8.25 -1 9 0 206.98 8.23 -1 9 0 223.75 8.15 -1 9 0 222.51 8.15 1 9 0 223.92 8.15 1 9 0 230.00 8.18 -3 -9 0 173.21 6.32 3 -9 0 164.41 6.17 -3 9 0 171.82 6.00 3 9 0 160.49 6.13 -3 9 0 152.69 6.02 -3 9 0 141.47 6.19 -5 -9 0 163.03 6.02 5 -9 0 157.60 6.10 -5 -9 0 161.46 6.35 -5 9 0 163.84 6.03 -5 9 0 155.50 6.00 5 9 0 164.19 6.08 -5 9 0 163.90 6.03 5 9 0 163.28 6.21 -7 -9 0 85.36 3.48 -7 -9 0 89.63 3.45 -7 -9 0 88.73 3.39 7 9 0 87.51 3.46 7 9 0 88.79 3.43 -7 9 0 93.70 3.49 -7 9 0 87.54 3.41 7 9 0 85.20 3.57 -9 -9 0 32.00 1.51 -9 -9 0 30.51 1.45 -9 -9 0 29.83 1.37 9 9 0 29.76 1.40 -9 9 0 31.76 1.37 -9 9 0 29.97 1.39 9 9 0 31.15 1.47 -11 -9 0 26.45 1.34 -11 -9 0 27.04 1.21 -11 -9 0 27.39 1.30 11 9 0 25.52 1.29 -11 9 0 26.41 1.22 11 9 0 26.95 1.20 -11 9 0 26.98 1.25 11 9 0 23.15 1.52 -13 -9 0 4.62 0.74 -13 -9 0 4.99 0.62 -13 -9 0 5.14 0.52 -13 9 0 4.66 0.63 13 9 0 5.41 0.52 -15 -9 0 45.15 1.81 -15 -9 0 47.75 1.85 0 -10 0 89.59 3.69 0 10 0 89.43 3.50 0 10 0 89.86 3.54 0 10 0 96.79 3.58 -2 -10 0 19.67 1.10 2 -10 0 20.52 1.29 -2 -10 0 21.59 1.34 -2 10 0 21.65 1.09 -2 10 0 21.02 1.02 2 10 0 20.69 1.05 -2 10 0 21.67 1.10 2 10 0 22.77 1.62 2 10 0 20.31 1.18 -4 -10 0 350.75 12.84 4 -10 0 349.15 12.72 -4 -10 0 346.26 12.62 -4 10 0 343.23 12.62 -4 10 0 337.63 12.66 4 10 0 342.94 12.64 4 10 0 352.89 12.85 4 10 0 344.91 12.69 -4 10 0 344.49 12.69 -6 -10 0 29.92 1.55 -6 -10 0 26.79 1.42 -6 10 0 26.19 1.27 -6 10 0 25.71 1.27 -8 -10 0 60.58 2.37 -8 -10 0 60.28 2.43 -8 10 0 59.21 2.40 8 10 0 57.96 2.38 8 10 0 57.85 2.42 -8 10 0 58.26 2.38 8 10 0 60.76 2.59 -10 -10 0 15.96 1.32 -10 -10 0 13.28 0.94 -10 -10 0 14.30 0.83 10 10 0 13.43 0.82 10 10 0 15.10 0.90 -10 10 0 15.01 0.86 -10 10 0 15.74 0.89 -12 -10 0 23.53 1.14 -12 -10 0 22.83 1.03 -12 -10 0 22.27 1.33 12 10 0 21.54 1.01 -12 10 0 22.54 1.09 -12 10 0 22.22 1.08 -14 -10 0 8.30 0.49 -14 -10 0 7.89 0.60 -1 11 0 90.94 3.56 -1 11 0 94.45 3.61 1 11 0 89.98 3.57 1 11 0 91.36 3.81 -3 -11 0 23.57 1.34 -3 -11 0 25.43 1.45 3 -11 0 25.57 1.37 -3 11 0 25.88 1.24 3 11 0 25.22 1.24 -3 11 0 22.26 1.16 3 11 0 24.03 1.19 3 11 0 25.77 1.58 -3 11 0 25.66 1.26 -5 -11 0 1.14 0.77 -5 -11 0 1.57 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2.18 -8 -4 20 0.11 0.42 8 -4 -20 0.46 0.35 8 4 -20 0.30 0.32 -8 4 20 0.23 0.32 8 4 -20 0.30 0.49 -8 4 20 0.35 0.62 -6 -4 20 30.32 1.37 -6 -4 20 31.64 1.62 6 -4 -20 31.54 1.32 -6 4 20 32.22 1.46 6 4 -20 30.90 1.32 6 4 -20 29.46 1.52 6 4 -20 31.52 1.42 4 -4 -20 14.93 0.97 4 -4 -20 13.08 0.74 -4 -4 20 13.70 1.03 4 4 -20 13.93 0.97 4 4 -20 14.02 0.73 -4 4 20 13.56 0.83 4 4 -20 14.76 0.86 2 -4 -20 26.93 1.12 2 -4 -20 25.65 1.19 -2 -4 20 26.12 1.36 2 4 -20 28.98 1.30 2 4 -20 26.31 1.20 -15 -5 20 11.39 0.90 15 -5 -20 13.48 0.79 -15 5 20 10.09 0.93 -15 5 20 12.22 0.65 -15 5 20 14.05 0.71 13 -5 -20 3.39 0.69 -13 -5 20 5.10 0.71 -13 5 20 4.42 0.84 13 5 -20 4.43 0.44 -13 5 20 4.26 0.43 -13 5 20 5.17 0.45 13 5 -20 6.34 1.13 -11 -5 20 26.68 1.29 11 -5 -20 25.66 1.11 11 -5 -20 27.36 1.43 11 5 -20 25.48 1.12 -11 5 20 25.61 1.12 -11 5 20 24.95 1.33 9 -5 -20 0.62 0.66 9 -5 -20 2.21 0.44 -9 -5 20 1.79 0.44 -9 5 20 2.58 0.51 9 5 -20 1.93 0.32 -9 5 20 2.25 0.45 -7 -5 20 36.24 1.54 7 -5 -20 36.86 1.47 -7 -5 20 35.51 1.73 -7 5 20 36.75 1.48 7 5 -20 32.81 1.69 -7 5 20 36.95 1.62 7 5 -20 35.57 1.47 -5 -5 20 3.44 0.77 5 -5 -20 4.29 0.45 5 5 -20 3.29 0.45 5 5 -20 4.19 0.75 -5 5 20 3.28 0.59 5 5 -20 3.47 0.57 -3 -5 20 48.37 2.04 3 -5 -20 46.97 1.90 3 -5 -20 46.34 1.83 3 5 -20 45.02 1.87 3 5 -20 48.42 1.89 -3 5 20 46.51 1.87 -14 -6 20 6.16 0.71 14 -6 -20 7.24 0.64 14 6 -20 7.82 0.86 -14 6 20 8.18 0.52 -14 6 20 6.70 0.87 -14 6 20 7.35 0.43 14 6 -20 5.69 0.45 -12 -6 20 1.39 0.38 12 -6 -20 1.29 0.43 -12 6 20 0.91 0.22 12 6 -20 1.49 0.25 -12 6 20 1.67 0.50 10 -6 -20 7.04 0.88 10 -6 -20 7.09 0.50 -10 -6 20 7.36 0.69 -10 6 20 7.96 0.79 10 6 -20 7.50 0.51 -10 6 20 6.41 0.50 -8 -6 20 2.77 0.39 8 -6 -20 2.62 0.42 8 -6 -20 4.81 1.00 -8 -6 20 2.43 0.64 -8 6 20 3.43 0.65 -8 6 20 2.85 0.43 8 6 -20 3.33 0.66 8 6 -20 2.92 0.41 -6 -6 20 4.15 0.73 6 -6 -20 3.58 0.40 -6 6 20 3.18 0.61 -6 6 20 4.06 0.57 6 6 -20 3.78 0.57 6 6 -20 3.34 0.40 4 -6 -20 18.11 0.80 -4 -6 20 18.83 1.04 4 6 -20 17.31 0.89 -4 6 20 18.63 0.88 4 6 -20 16.73 0.90 11 -7 -20 0.08 0.47 -11 -7 20 0.30 0.32 11 7 -20 0.07 0.18 -11 7 20 0.51 0.48 -11 7 20 0.16 0.22 9 -7 -20 0.74 0.26 9 -7 -20 0.62 0.46 -9 -7 20 0.73 0.31 -9 7 20 0.86 0.39 9 7 -20 0.79 0.19 -9 7 20 1.19 0.25 -7 -7 20 5.14 0.69 7 -7 -20 5.46 0.43 -7 7 20 4.81 0.58 7 7 -20 5.06 0.41 7 7 -20 4.61 0.66 5 -7 -20 3.33 0.36 -5 -7 20 4.52 0.80 -5 7 20 3.19 0.35 -5 7 20 4.86 0.64 5 7 -20 2.80 0.54 -16 0 21 -0.11 0.25 16 0 -21 -0.05 0.38 -16 0 21 0.10 0.69 14 0 -21 -0.45 0.51 -14 0 21 0.42 0.46 14 0 -21 0.20 0.29 -12 0 21 0.17 0.45 12 0 -21 0.36 0.66 -10 0 21 0.12 0.47 10 0 -21 0.08 0.29 -10 0 21 -0.11 0.33 -8 0 21 -0.11 0.33 -8 0 21 -0.32 0.45 8 0 -21 0.14 0.53 8 0 -21 -0.04 0.32 6 0 -21 0.48 0.39 -6 0 21 -0.44 0.37 -6 0 21 0.06 0.31 6 0 -21 0.13 0.27 6 0 -21 -0.16 0.55 4 0 -21 0.13 0.53 4 0 -21 -0.19 0.46 4 0 -21 0.18 0.26 -4 0 21 -0.24 0.27 2 0 -21 0.21 0.31 2 0 -21 -0.27 0.28 -2 0 21 -0.18 0.23 -15 -1 21 2.72 0.55 15 -1 -21 3.04 0.53 -15 1 21 2.62 0.56 15 1 -21 3.04 0.55 -15 1 21 1.94 0.42 -13 -1 21 -0.03 0.52 13 -1 -21 0.08 0.52 13 -1 -21 -0.08 0.27 -13 1 21 0.76 0.51 13 1 -21 0.53 0.67 13 1 -21 0.03 0.27 11 -1 -21 2.21 0.76 -11 -1 21 3.82 0.84 11 -1 -21 3.57 0.50 -11 -1 21 3.81 0.78 11 1 -21 3.08 0.48 -11 1 21 3.30 0.58 9 -1 -21 12.60 0.71 -9 -1 21 11.59 0.89 -9 -1 21 11.84 1.07 -9 1 21 12.48 0.92 -9 1 21 10.75 1.45 9 1 -21 11.84 0.71 7 -1 -21 2.34 0.56 7 -1 -21 1.97 0.32 -7 -1 21 1.81 0.43 -7 -1 21 1.42 0.35 -7 1 21 1.34 0.38 7 1 -21 2.00 0.85 7 1 -21 1.27 0.29 -7 1 21 2.28 0.48 5 -1 -21 3.66 0.49 5 -1 -21 4.32 0.83 -5 -1 21 3.46 0.80 -5 -1 21 2.66 0.55 5 -1 -21 4.03 0.89 5 1 -21 3.34 0.49 -5 1 21 3.89 0.59 -5 1 21 2.90 0.83 5 1 -21 3.94 0.63 5 1 -21 3.94 0.63 3 -1 -21 13.97 0.71 -3 -1 21 13.74 0.94 3 -1 -21 13.75 0.83 3 1 -21 14.41 0.83 3 1 -21 14.27 0.71 -3 1 21 13.42 0.98 1 -1 -21 10.45 0.54 -1 -1 21 8.83 0.81 1 -1 -21 11.01 0.65 1 1 -21 10.64 0.66 -1 1 21 10.57 0.85 -16 -2 21 0.22 0.53 16 -2 -21 0.30 0.34 -16 2 21 -0.03 0.22 -16 2 21 0.85 0.57 16 2 -21 0.11 0.50 14 -2 -21 24.82 1.32 -14 -2 21 22.43 1.25 -14 2 21 24.24 1.30 14 2 -21 22.25 1.04 -14 2 21 27.81 1.17 14 2 -21 25.42 1.35 12 -2 -21 2.26 0.66 -12 -2 21 1.13 0.44 12 -2 -21 1.43 0.31 12 2 -21 2.42 0.46 12 2 -21 2.61 0.77 -12 2 21 1.49 0.47 10 -2 -21 24.83 1.10 -10 -2 21 24.79 1.40 -10 -2 21 24.50 1.25 10 2 -21 25.13 1.11 -10 2 21 24.58 1.29 8 -2 -21 0.16 0.25 -8 -2 21 0.06 0.30 -8 -2 21 -0.45 0.36 -8 2 21 -0.38 0.40 8 2 -21 0.11 0.74 8 2 -21 -0.17 0.27 -6 -2 21 72.71 2.99 6 -2 -21 80.17 2.96 -6 -2 21 70.44 2.79 6 -2 -21 71.67 2.76 6 2 -21 69.39 2.91 -6 2 21 71.34 2.83 6 2 -21 70.16 2.75 6 2 -21 73.70 2.85 -4 -2 21 3.49 0.75 4 -2 -21 3.20 0.63 4 -2 -21 3.08 0.45 4 2 -21 4.91 0.98 -4 2 21 3.33 0.59 -4 2 21 2.84 0.89 4 2 -21 3.03 0.45 4 2 -21 2.58 0.46 2 -2 -21 33.73 1.37 2 -2 -21 28.94 1.32 -2 -2 21 32.76 1.52 2 2 -21 34.90 1.38 -2 2 21 31.09 1.55 2 2 -21 33.32 1.33 15 -3 -21 1.29 0.44 -15 -3 21 1.41 0.44 15 3 -21 1.74 0.59 -15 3 21 2.28 0.67 -15 3 21 1.29 0.22 -15 3 21 0.95 0.25 13 -3 -21 6.53 0.88 -13 -3 21 7.48 0.78 -13 3 21 7.12 0.83 13 3 -21 6.28 0.51 -13 3 21 6.81 0.85 11 -3 -21 79.32 3.24 11 -3 -21 81.02 3.01 -11 -3 21 76.62 3.12 -11 3 21 79.06 3.14 11 3 -21 81.97 3.02 9 -3 -21 15.46 0.77 -9 -3 21 15.49 1.09 -9 -3 21 14.60 0.93 9 3 -21 15.31 0.79 -9 3 21 15.03 0.96 -7 -3 21 30.50 1.56 7 -3 -21 31.35 1.28 -7 -3 21 29.14 1.34 7 3 -21 31.73 1.29 -7 3 21 30.01 1.40 5 -3 -21 2.04 0.40 5 -3 -21 1.67 0.43 -5 -3 21 1.05 0.30 5 3 -21 1.26 0.26 -5 3 21 1.67 0.37 5 3 -21 1.76 0.45 3 -3 -21 27.02 1.09 -3 -3 21 25.40 1.30 3 -3 -21 24.87 1.18 3 3 -21 26.79 1.18 3 3 -21 26.18 1.17 14 -4 -21 1.50 0.45 -14 -4 21 1.31 0.39 -14 4 21 0.99 0.30 14 4 -21 0.95 0.29 -14 4 21 0.92 0.63 14 4 -21 1.41 0.55 12 -4 -21 10.73 0.93 12 -4 -21 11.58 0.75 -12 -4 21 11.30 0.81 -12 4 21 11.61 0.71 12 4 -21 9.74 0.59 -12 4 21 10.02 0.87 10 -4 -21 11.25 1.16 10 -4 -21 12.00 0.67 -10 -4 21 12.08 0.83 -10 -4 21 12.54 0.95 -10 4 21 12.18 0.88 10 4 -21 12.55 0.67 -8 -4 21 0.46 0.35 8 -4 -21 1.32 0.28 -8 4 21 0.86 0.38 8 4 -21 2.07 0.47 8 4 -21 1.05 0.28 6 -4 -21 3.48 0.41 -6 -4 21 4.58 0.73 6 4 -21 3.17 0.44 -6 4 21 4.10 0.59 6 4 -21 4.09 0.45 4 -4 -21 10.95 0.57 -4 -4 21 10.43 0.83 4 -4 -21 11.83 0.88 4 4 -21 10.04 0.59 -4 4 21 8.42 0.76 4 4 -21 11.78 0.68 13 -5 -21 5.02 0.84 -13 5 21 4.30 0.40 13 5 -21 3.95 0.44 -11 -5 21 23.60 1.10 11 -5 -21 21.73 1.14 -11 5 21 21.81 1.17 11 5 -21 23.64 0.98 9 -5 -21 0.05 0.22 -9 -5 21 0.25 0.33 9 -5 -21 -0.04 0.77 -9 -5 21 -0.02 0.23 9 5 -21 -0.12 0.21 -9 5 21 0.12 0.33 -9 5 21 -0.17 0.34 -7 -5 21 1.56 0.44 7 -5 -21 1.11 0.23 7 5 -21 1.97 0.39 -7 5 21 1.12 0.35 7 5 -21 1.20 0.24 -5 -5 21 0.36 0.20 5 -5 -21 0.43 0.19 5 5 -21 0.56 0.29 -5 5 21 0.34 0.34 5 5 -21 0.50 0.28 10 -6 -21 -0.43 0.43 -10 -6 21 0.83 0.33 10 -6 -21 0.20 0.21 10 6 -21 0.26 0.18 -10 6 21 0.41 0.39 -10 6 21 0.28 0.19 -8 -6 21 5.71 0.52 -8 -6 21 7.65 0.69 8 -6 -21 7.39 0.48 -8 6 21 7.59 0.46 8 6 -21 6.17 0.44 -8 6 21 6.96 0.60 -14 0 22 37.02 1.57 14 0 -22 29.16 1.67 14 0 -22 38.34 1.52 12 0 -22 -0.10 0.22 12 0 -22 -0.28 0.84 -12 0 22 0.04 0.35 10 0 -22 41.69 1.58 -10 0 22 41.95 1.73 -10 0 22 34.69 1.99 -8 0 22 1.21 0.35 8 0 -22 1.04 0.27 6 0 -22 47.79 1.88 -6 0 22 49.89 1.95 6 0 -22 46.46 1.95 -6 0 22 49.56 2.09 4 0 -22 25.00 1.04 4 0 -22 26.00 1.09 -4 0 22 20.59 1.62 -15 -1 22 3.80 0.76 15 1 -22 3.35 0.56 -15 1 22 4.78 0.72 13 -1 -22 7.15 1.17 13 -1 -22 6.72 0.60 -13 -1 22 3.86 0.96 -13 -1 22 4.76 0.68 -13 1 22 5.04 0.71 13 1 -22 5.92 0.94 13 1 -22 5.18 0.47 11 -1 -22 7.40 0.52 -11 -1 22 6.21 0.88 -11 -1 22 7.21 0.72 -11 1 22 6.39 0.72 11 1 -22 6.64 0.50 9 -1 -22 7.41 0.53 -9 -1 22 7.01 0.69 -9 -1 22 8.48 0.90 9 1 -22 8.54 0.62 -9 1 22 7.63 0.68 7 -1 -22 49.47 1.83 -7 -1 22 48.18 2.04 -7 -1 22 47.87 1.86 -7 1 22 40.49 2.15 7 1 -22 45.69 1.91 7 1 -22 46.05 1.83 -7 1 22 49.77 1.88 5 -1 -22 0.02 0.20 -5 -1 22 0.05 0.20 5 -1 -22 0.02 0.37 5 1 -22 0.27 0.20 -5 1 22 0.33 0.37 5 1 -22 0.09 0.33 -14 -2 22 1.00 0.27 -14 -2 22 1.20 0.37 14 -2 -22 0.96 0.57 14 2 -22 0.52 0.51 -12 -2 22 5.43 0.81 12 -2 -22 6.07 0.48 -12 -2 22 6.71 0.65 -12 2 22 6.18 0.71 12 2 -22 5.76 0.46 -10 -2 22 1.49 0.35 -10 -2 22 1.34 0.34 10 2 -22 1.83 0.39 -8 -2 22 0.25 0.32 8 -2 -22 0.49 0.21 -8 -2 22 0.26 0.24 -8 2 22 0.31 0.35 8 2 -22 -0.04 0.24 6 -2 -22 13.66 0.69 -6 -2 22 15.25 0.95 6 2 -22 13.50 0.81 -6 2 22 14.28 0.80 6 2 -22 14.57 0.70 -4 -2 22 4.82 0.75 4 -2 -22 5.66 0.49 4 2 -22 3.90 0.52 4 2 -22 3.97 0.38 13 -3 -22 9.04 1.02 -13 3 22 9.43 0.80 13 3 -22 6.77 0.56 13 3 -22 7.42 0.87 11 -3 -22 5.53 0.45 11 -3 -22 6.97 0.98 -11 -3 22 4.76 0.74 -11 -3 22 5.03 0.60 -11 3 22 6.13 0.66 11 3 -22 4.92 0.43 -9 -3 22 1.40 0.34 9 -3 -22 1.83 0.35 9 3 -22 1.33 0.24 -9 3 22 1.91 0.37 7 -3 -22 8.13 0.51 -7 -3 22 9.94 0.75 -7 -3 22 8.47 0.77 7 3 -22 8.92 0.53 -7 3 22 8.86 0.63 5 -3 -22 0.57 0.20 -5 -3 22 0.20 0.25 5 3 -22 0.22 0.25 5 3 -22 0.66 0.37 12 -4 -22 26.63 1.28 12 -4 -22 23.53 1.16 -12 -4 22 27.18 1.36 -12 -4 22 26.56 1.19 12 4 -22 28.28 1.25 -12 4 22 28.72 1.36 10 -4 -22 0.27 0.20 -10 -4 22 0.01 0.19 -10 -4 22 0.47 0.31 10 4 -22 0.18 0.19 -10 4 22 -0.14 0.27 -8 -4 22 1.06 0.41 8 -4 -22 0.28 0.19 -8 -4 22 0.48 0.25 8 4 -22 0.33 0.19 10 0 -23 0.20 0.18 -10 0 23 -0.19 0.29 8 0 -23 -0.09 0.20 -8 0 23 0.06 0.24 -8 0 23 -0.39 0.35 -11 -1 23 4.94 0.65 -11 -1 23 5.88 0.66 -11 1 23 6.58 0.58 11 1 -23 6.78 0.47 -9 -1 23 2.62 0.58 9 -1 -23 2.55 0.33 9 1 -23 2.26 0.30 -9 1 23 3.13 0.63 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 39990 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Br1 Br 0.13227(2) 0.10413(3) 0.24381(2) 0.03490(15) Uani 1 1 d . . C1 C 0.21473(18) 0.1567(2) 0.34067(17) 0.0240(6) Uani 1 1 d . . C2 C 0.25222(18) 0.2562(2) 0.34315(16) 0.0221(6) Uani 1 1 d . . H2A H 0.2359 0.2992 0.2977 0.026 Uiso 1 1 calc R U C3 C 0.31372(18) 0.2891(2) 0.41411(17) 0.0203(6) Uani 1 1 d . . C4 C 0.33665(17) 0.2262(2) 0.48082(16) 0.0200(6) Uani 1 1 d . . C5 C 0.29824(18) 0.1285(2) 0.47855(17) 0.0226(6) Uani 1 1 d . . H5A H 0.3136 0.0865 0.5243 0.027 Uiso 1 1 calc R U C6 C 0.23634(19) 0.0941(2) 0.40677(19) 0.0249(6) Uani 1 1 d . . H6A H 0.2087 0.0275 0.4030 0.030 Uiso 1 1 calc R U C7 C 0.36601(19) 0.3909(2) 0.43706(18) 0.0234(6) Uani 1 1 d . . C8 C 0.42072(19) 0.3739(2) 0.52649(17) 0.0238(6) Uani 1 1 d . . C9 C 0.3135(2) 0.4880(2) 0.42261(17) 0.0266(6) Uani 1 1 d . . C10 C 0.2671(2) 0.5634(2) 0.40908(19) 0.0296(7) Uani 1 1 d . . C11 C 0.2103(2) 0.6536(2) 0.39000(19) 0.0303(7) Uani 1 1 d . . C12 C 0.1938(3) 0.7148(3) 0.3248(2) 0.0439(9) Uani 1 1 d . . H12A H 0.2201 0.6974 0.2930 0.053 Uiso 1 1 calc R U C13 C 0.1392(3) 0.8014(3) 0.3051(3) 0.0556(11) Uani 1 1 d . . H13A H 0.1280 0.8424 0.2597 0.067 Uiso 1 1 calc R U C14 C 0.1015(2) 0.8281(3) 0.3509(3) 0.0499(10) Uani 1 1 d . . H14A H 0.0648 0.8882 0.3377 0.060 Uiso 1 1 calc R U C15 C 0.1168(3) 0.7675(4) 0.4159(3) 0.0617(12) Uani 1 1 d . . H15A H 0.0900 0.7853 0.4472 0.074 Uiso 1 1 calc R U C16 C 0.1714(3) 0.6805(3) 0.4361(3) 0.0523(10) Uani 1 1 d . . H16A H 0.1821 0.6394 0.4813 0.063 Uiso 1 1 calc R U C17 C 0.43870(18) 0.2310(2) 0.62409(16) 0.0240(6) Uani 1 1 d . . H17A H 0.3948 0.2066 0.6384 0.029 Uiso 1 1 calc R U H17B H 0.4722 0.2871 0.6619 0.029 Uiso 1 1 calc R U C18 C 0.4945(2) 0.1371(3) 0.62965(18) 0.0282(6) Uani 1 1 d . . C19 C 0.5617(3) 0.1517(3) 0.6135(3) 0.0535(11) Uani 1 1 d . . H19A H 0.5719 0.2203 0.5976 0.064 Uiso 1 1 calc R U C20 C 0.6143(4) 0.0658(4) 0.6206(4) 0.0825(19) Uani 1 1 d . . H20A H 0.6611 0.0759 0.6106 0.099 Uiso 1 1 calc R U C21 C 0.5982(4) -0.0349(4) 0.6425(4) 0.0777(17) Uani 1 1 d . . H21A H 0.6325 -0.0944 0.6446 0.093 Uiso 1 1 calc R U C22 C 0.5338(3) -0.0489(4) 0.6608(3) 0.0634(13) Uani 1 1 d . . H22A H 0.5243 -0.1172 0.6776 0.076 Uiso 1 1 calc R U C23 C 0.4818(2) 0.0380(3) 0.6548(2) 0.0437(9) Uani 1 1 d . . H23A H 0.4373 0.0287 0.6682 0.052 Uiso 1 1 calc R U N1 N 0.39906(15) 0.27779(18) 0.54602(14) 0.0214(5) Uani 1 1 d . . O1 O 0.41836(14) 0.39352(16) 0.39959(13) 0.0291(5) Uani 1 1 d . . H1A H 0.4480 0.4493 0.4131 0.044 Uiso 1 1 calc R U O2 O 0.47463(15) 0.43436(18) 0.57048(13) 0.0333(5) Uani 1 1 d . . 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 0.0311(2) 0.0339(2) 0.0309(2) -0.00905(12) 0.00620(16) -0.00614(13) C1 0.0219(15) 0.0207(14) 0.0298(15) -0.0057(11) 0.0118(12) -0.0006(11) C2 0.0229(15) 0.0190(13) 0.0254(14) -0.0005(11) 0.0119(12) 0.0027(11) C3 0.0225(15) 0.0155(12) 0.0272(14) -0.0010(10) 0.0150(12) 0.0008(10) C4 0.0191(14) 0.0185(13) 0.0248(14) -0.0022(10) 0.0119(12) 0.0020(10) C5 0.0242(15) 0.0171(12) 0.0291(15) 0.0010(11) 0.0142(13) -0.0009(11) C6 0.0242(16) 0.0169(13) 0.0375(17) -0.0034(11) 0.0174(14) -0.0024(11) C7 0.0273(16) 0.0195(14) 0.0266(15) -0.0021(11) 0.0150(13) -0.0041(11) C8 0.0258(16) 0.0217(13) 0.0273(15) -0.0026(11) 0.0149(13) -0.0023(12) C9 0.0360(17) 0.0192(14) 0.0274(15) -0.0006(11) 0.0168(13) -0.0036(12) C10 0.0382(18) 0.0215(15) 0.0335(16) -0.0002(12) 0.0199(15) -0.0020(13) C11 0.0364(18) 0.0182(14) 0.0366(17) -0.0030(12) 0.0167(15) 0.0007(12) C12 0.057(2) 0.0350(19) 0.048(2) 0.0087(16) 0.032(2) 0.0129(17) C13 0.068(3) 0.037(2) 0.059(3) 0.0162(18) 0.026(2) 0.0187(19) C14 0.037(2) 0.0295(18) 0.070(3) -0.0043(17) 0.0123(19) 0.0088(15) C15 0.068(3) 0.051(2) 0.082(3) -0.003(2) 0.048(3) 0.018(2) C16 0.073(3) 0.044(2) 0.056(2) 0.0081(18) 0.043(2) 0.017(2) C17 0.0222(15) 0.0284(15) 0.0228(14) -0.0002(11) 0.0114(12) 0.0023(12) C18 0.0275(16) 0.0315(15) 0.0266(15) 0.0020(12) 0.0130(13) 0.0072(13) C19 0.057(3) 0.045(2) 0.081(3) 0.011(2) 0.050(3) 0.0150(19) C20 0.089(4) 0.066(3) 0.139(5) 0.024(3) 0.092(4) 0.034(3) C21 0.084(4) 0.059(3) 0.114(5) 0.024(3) 0.066(4) 0.042(3) C22 0.060(3) 0.041(2) 0.088(3) 0.027(2) 0.032(3) 0.020(2) C23 0.038(2) 0.041(2) 0.057(2) 0.0194(17) 0.0253(18) 0.0127(16) N1 0.0208(12) 0.0196(11) 0.0232(12) -0.0012(9) 0.0095(10) -0.0021(9) O1 0.0333(12) 0.0266(11) 0.0358(12) -0.0060(8) 0.0230(11) -0.0085(9) O2 0.0337(13) 0.0309(11) 0.0315(11) -0.0063(9) 0.0114(10) -0.0141(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 C6 C1 C2 122.2(3) C6 C1 Br1 118.6(2) C2 C1 Br1 119.2(2) C3 C2 C1 117.1(3) C2 C3 C4 121.2(3) C2 C3 C7 130.6(3) C4 C3 C7 108.2(2) C5 C4 C3 121.7(3) C5 C4 N1 127.8(3) C3 C4 N1 110.5(2) C4 C5 C6 117.5(3) C1 C6 C5 120.3(3) O1 C7 C9 113.4(2) O1 C7 C3 109.6(2) C9 C7 C3 111.6(3) O1 C7 C8 109.3(2) C9 C7 C8 110.4(2) C3 C7 C8 101.9(2) O2 C8 N1 126.0(3) O2 C8 C7 126.2(3) N1 C8 C7 107.8(2) C10 C9 C7 176.4(3) C9 C10 C11 178.1(3) C12 C11 C16 118.8(3) C12 C11 C10 119.7(3) C16 C11 C10 121.5(3) C11 C12 C13 120.8(4) C14 C13 C12 120.2(4) C13 C14 C15 119.8(4) C14 C15 C16 120.4(4) C15 C16 C11 120.0(4) N1 C17 C18 112.4(2) C23 C18 C19 119.5(3) C23 C18 C17 120.4(3) C19 C18 C17 120.0(3) C18 C19 C20 119.9(4) C19 C20 C21 119.8(4) C22 C21 C20 120.5(4) C21 C22 C23 119.5(4) C18 C23 C22 120.7(4) C8 N1 C4 111.5(2) C8 N1 C17 124.4(2) C4 N1 C17 123.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C1 1.896(3) C1 C6 1.387(4) C1 C2 1.396(4) C2 C3 1.373(4) C3 C4 1.395(4) C3 C7 1.516(4) C4 C5 1.386(4) C4 N1 1.403(4) C5 C6 1.391(4) C7 O1 1.417(3) C7 C9 1.476(4) C7 C8 1.562(4) C8 O2 1.214(4) C8 N1 1.359(4) C9 C10 1.200(5) C10 C11 1.446(4) C11 C12 1.377(5) C11 C16 1.392(5) C12 C13 1.386(5) C13 C14 1.370(6) C14 C15 1.375(7) C15 C16 1.389(6) C17 N1 1.460(4) C17 C18 1.508(4) C18 C23 1.378(5) C18 C19 1.386(5) C19 C20 1.387(6) C20 C21 1.389(7) C21 C22 1.362(7) C22 C23 1.395(6) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A O2 0.84 1.93 2.753(3) 167.7 5_666 C17 H17B Br1 0.99 2.91 3.784(3) 148.0 8_556 O1 H1A O2 0.84 1.93 2.753(3) 167.7 5_666 C17 H17B Br1 0.99 2.91 3.784(3) 148.0 8_556 C17 H17B Br1 0.99 2.91 3.784(3) 148.0 8_556 O1 H1A O2 0.84 1.93 2.753(3) 167.7 5_666 C17 H17B Br1 0.99 2.91 3.784(3) 148.0 8_556 O1 H1A O2 0.84 1.93 2.753(3) 167.7 5_666