#------------------------------------------------------------------------------ #$Date: 2025-08-21 23:24:23 +0100 (Thu, 21 Aug 2025) $ #$Revision: 301857 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/22/7112255.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_7112255 loop_ _publ_author_name 'Min Zhang' 'Xiaoming Zhao' 'Shengcai Zheng' _publ_section_title ; Enantioselective domino reaction of CO2, amines and allyl chlorides under iridium catalysis: formation of allyl carbamates ; _journal_name_full Chem.Commun. _journal_page_first 4455 _journal_paper_doi 10.1039/C4CC00413B _journal_volume 50 _journal_year 2014 _chemical_formula_sum 'C13 H16 Br N O2' _chemical_formula_weight 298.18 _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 9.4480(7) _cell_length_b 14.9400(10) _cell_length_c 28.8691(15) _cell_measurement_reflns_used 8854 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 68.16 _cell_measurement_theta_min 3.06 _cell_volume 4075.0(5) _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-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0676 _diffrn_reflns_av_unetI/netI 0.0778 _diffrn_reflns_Laue_measured_fraction_full 0.958 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 17237 _diffrn_reflns_point_group_measured_fraction_full 0.942 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 67.990 _diffrn_reflns_theta_min 3.061 _exptl_absorpt_coefficient_mu 4.052 _exptl_absorpt_correction_T_max 0.753 _exptl_absorpt_correction_T_min 0.219 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.458 _exptl_crystal_description rod _exptl_crystal_F_000 1824 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.353 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.199 _refine_ls_abs_structure_details ; Flack x determined using 2421 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.145(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 466 _refine_ls_number_reflns 6977 _refine_ls_number_restraints 72 _refine_ls_restrained_S_all 1.124 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.1024 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1032P)^2^+46.5625P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2680 _refine_ls_wR_factor_ref 0.2743 _reflns_Friedel_coverage 0.745 _reflns_Friedel_fraction_full 0.920 _reflns_Friedel_fraction_max 0.917 _reflns_number_gt 6253 _reflns_number_total 6977 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc00413b2.cif _cod_data_source_block cu_30926b _cod_database_code 7112255 #BEGIN Tags that were not found in dictionaries: _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 0.195 _shelx_estimated_absorpt_t_max 0.793 _shelxl_version_number 2013-2 _shelx_res_file ; TITL cu_30926b in P2(1)2(1)2(1) CELL 1.54178 9.4480 14.9400 28.8691 90.000 90.000 90.000 ZERR 12.00 0.0007 0.0010 0.0015 0.000 0.000 0.000 LATT -1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O Br UNIT 156 192 12 24 12 OMIT -2.00 136.00 L.S. 4 ACTA BOND FMAP 2 PLAN 10 SIZE 0.06 0.06 0.60 ISOR 0.005 O1, O2, N2, C8, C23, N3, O5, O6, C27, C31, C36 ISOR 0.002 O4 CONF EQIV $1 x-1/2, -y+1/2, -z+1 HTAB N1 O4_$1 EQIV $2 -x+3/2, -y+2, z+1/2 HTAB N2 O6_$2 EQIV $3 -x+1, y+1/2, -z+1/2 HTAB N3 O2_$3 TEMP 23.000 WGHT 0.103200 46.562500 FVAR 0.07014 MOLE 1 BR1 5 0.431500 0.048173 0.150318 11.00000 0.06259 0.06141 = 0.04350 -0.00393 0.01285 -0.00772 N1 3 0.397504 0.006437 0.439525 11.00000 0.01809 0.01098 = 0.04220 -0.00205 -0.00935 -0.00128 AFIX 43 H1 2 0.372870 -0.048038 0.434264 11.00000 -1.20000 AFIX 0 O1 4 0.263241 0.039465 0.378568 11.00000 0.03103 0.01420 = 0.02965 0.00532 -0.01298 -0.00158 O2 4 0.367532 0.152194 0.418426 11.00000 0.06445 0.00747 = 0.05049 0.00119 -0.01873 -0.00194 C1 1 0.249022 0.089137 0.299764 11.00000 0.01803 0.01856 = 0.02880 0.00429 -0.00227 -0.00326 C2 1 0.177386 0.118317 0.261633 11.00000 0.05425 0.03862 = 0.03390 -0.00020 -0.01166 0.02611 AFIX 43 H2 2 0.089766 0.145532 0.265772 11.00000 -1.20000 AFIX 0 C3 1 0.229247 0.109236 0.217092 11.00000 0.02524 0.05439 = 0.03367 0.01090 -0.00468 0.00476 AFIX 43 H3 2 0.178834 0.132833 0.192264 11.00000 -1.20000 AFIX 0 C4 1 0.357592 0.064574 0.209209 11.00000 0.01360 0.02329 = 0.05303 0.00673 -0.00270 -0.00474 C5 1 0.432391 0.034643 0.247837 11.00000 0.01504 0.03536 = 0.04200 0.00777 0.00755 0.00948 AFIX 43 H5 2 0.518601 0.005702 0.243661 11.00000 -1.20000 AFIX 0 C6 1 0.381882 0.046888 0.291562 11.00000 0.03897 0.03427 = 0.03701 0.00383 -0.00458 0.01218 AFIX 43 H6 2 0.435311 0.027232 0.316633 11.00000 -1.20000 AFIX 0 C7 1 0.191324 0.101809 0.348209 11.00000 0.04302 0.01490 = 0.02855 0.00294 -0.00701 0.01332 AFIX 13 H7 2 0.218814 0.162083 0.358132 11.00000 -1.20000 AFIX 0 C8 1 0.034159 0.096064 0.352913 11.00000 0.02835 0.03476 = 0.03877 0.00605 0.00145 0.01316 AFIX 43 H8 2 -0.021152 0.136815 0.336623 11.00000 -1.20000 AFIX 0 C9 1 -0.029155 0.036966 0.378630 11.00000 0.01668 0.07763 = 0.06180 -0.00195 -0.00698 -0.00460 AFIX 93 H9A 2 0.023807 -0.004514 0.395259 11.00000 -1.20000 H9B 2 -0.127430 0.036151 0.380406 11.00000 -1.20000 AFIX 0 C10 1 0.341958 0.073505 0.413595 11.00000 0.03331 0.00490 = 0.02396 -0.00147 -0.00333 0.00301 C11 1 0.498201 0.026029 0.476076 11.00000 0.01959 0.02552 = 0.03519 -0.01041 -0.00720 -0.00127 AFIX 13 H11 2 0.464104 0.077972 0.493547 11.00000 -1.20000 AFIX 0 C12 1 0.509232 -0.052348 0.508551 11.00000 0.07233 0.03535 = 0.05365 0.01282 -0.03159 -0.01441 AFIX 137 H12A 2 0.419530 -0.062008 0.523348 11.00000 -1.50000 H12B 2 0.579852 -0.040191 0.531617 11.00000 -1.50000 H12C 2 0.535358 -0.104886 0.491419 11.00000 -1.50000 AFIX 0 C13 1 0.645561 0.047555 0.456878 11.00000 0.04569 0.04524 = 0.06850 0.01793 0.00280 -0.00519 AFIX 137 H13A 2 0.675771 0.000040 0.436793 11.00000 -1.50000 H13B 2 0.711290 0.053504 0.482050 11.00000 -1.50000 H13C 2 0.641926 0.102604 0.439768 11.00000 -1.50000 AFIX 0 BR2 5 0.812011 0.771033 0.854617 11.00000 0.05913 0.07696 = 0.03981 -0.00866 -0.00803 0.02188 N2 3 0.875543 0.829109 0.556932 11.00000 0.02872 0.01848 = 0.02883 0.00092 0.00481 0.00572 AFIX 43 H2A 2 0.850554 0.883245 0.562904 11.00000 -1.20000 AFIX 0 O3 4 0.748423 0.792679 0.619554 11.00000 0.03575 0.00849 = 0.03962 -0.00361 0.01674 -0.00346 O4 4 0.845690 0.682047 0.574520 11.00000 0.04294 0.01848 = 0.03429 0.00087 0.00980 0.00871 C14 1 0.708698 0.739029 0.697954 11.00000 0.02277 0.01193 = 0.03810 0.00200 0.00716 -0.00457 C15 1 0.704927 0.664268 0.726989 11.00000 0.05616 0.01840 = 0.04066 -0.00254 -0.00689 0.00675 AFIX 43 H15 2 0.681442 0.608268 0.715206 11.00000 -1.20000 AFIX 0 C16 1 0.736732 0.674575 0.773761 11.00000 0.06878 0.02740 = 0.03888 0.00596 0.01289 0.00763 AFIX 43 H16 2 0.738480 0.624557 0.792930 11.00000 -1.20000 AFIX 0 C17 1 0.766138 0.759079 0.792405 11.00000 0.02771 0.03775 = 0.03848 -0.00179 0.00114 0.01283 C18 1 0.768970 0.831100 0.762588 11.00000 0.04526 0.03099 = 0.04386 -0.01031 0.00446 -0.01446 AFIX 43 H18 2 0.793806 0.887097 0.774074 11.00000 -1.20000 AFIX 0 C19 1 0.735951 0.822660 0.716015 11.00000 0.06917 0.00758 = 0.04613 -0.00070 0.01492 -0.00913 AFIX 43 H19 2 0.732218 0.873010 0.697112 11.00000 -1.20000 AFIX 0 C20 1 0.673600 0.725156 0.646596 11.00000 0.04299 0.01383 = 0.03468 0.00009 0.01078 -0.01210 AFIX 13 H20 2 0.704571 0.665392 0.636949 11.00000 -1.20000 AFIX 0 C21 1 0.521701 0.734654 0.638055 11.00000 0.02120 0.03080 = 0.04309 -0.00426 -0.00151 -0.01010 AFIX 43 H21 2 0.462724 0.699181 0.656172 11.00000 -1.20000 AFIX 0 C22 1 0.458787 0.786591 0.608246 11.00000 0.04179 0.06748 = 0.04705 0.00544 -0.00500 -0.01169 AFIX 93 H22A 2 0.512068 0.823668 0.589127 11.00000 -1.20000 H22B 2 0.360577 0.786605 0.606078 11.00000 -1.20000 AFIX 0 C23 1 0.826967 0.761494 0.582567 11.00000 0.01791 0.00489 = 0.02396 -0.00048 0.00379 0.00366 C24 1 0.972197 0.809911 0.518400 11.00000 0.03533 0.01937 = 0.02700 -0.00307 0.00795 0.01197 AFIX 13 H24 2 0.944080 0.753412 0.503813 11.00000 -1.20000 AFIX 0 C25 1 1.126943 0.801498 0.535884 11.00000 0.01253 0.07363 = 0.05758 -0.00318 -0.00527 0.00567 AFIX 137 H25A 2 1.158544 0.858414 0.547342 11.00000 -1.50000 H25B 2 1.186817 0.782872 0.510805 11.00000 -1.50000 H25C 2 1.131200 0.758002 0.560321 11.00000 -1.50000 AFIX 0 C26 1 0.959121 0.884810 0.483190 11.00000 0.11587 0.02340 = 0.03926 0.00784 0.01740 0.00773 AFIX 137 H26A 2 0.867154 0.882680 0.469094 11.00000 -1.50000 H26B 2 1.030439 0.877744 0.459787 11.00000 -1.50000 H26C 2 0.971496 0.941410 0.498402 11.00000 -1.50000 AFIX 0 BR3 5 0.617137 0.842737 0.344400 11.00000 0.05790 0.07280 = 0.05148 0.01511 0.00781 0.01421 N3 3 0.594320 0.833084 0.050022 11.00000 0.02869 0.01177 = 0.03698 0.00419 -0.00901 0.00062 AFIX 43 H3A 2 0.606842 0.777318 0.056166 11.00000 -1.20000 AFIX 0 O5 4 0.729063 0.854539 0.111632 11.00000 0.03293 0.01542 = 0.04017 0.00219 -0.00932 -0.00184 O6 4 0.655454 0.975554 0.070419 11.00000 0.03337 0.00882 = 0.04089 0.00288 -0.00685 0.00173 C27 1 0.764881 0.889065 0.191482 11.00000 0.03398 0.02100 = 0.03134 0.00241 -0.00492 -0.00118 C28 1 0.836838 0.928822 0.227703 11.00000 0.01869 0.02358 = 0.05280 0.00821 -0.01564 -0.00349 AFIX 43 H28 2 0.915087 0.964483 0.221270 11.00000 -1.20000 AFIX 0 C29 1 0.795339 0.916941 0.273653 11.00000 0.01553 0.02666 = 0.04897 -0.00282 -0.00592 -0.00157 AFIX 43 H29 2 0.843271 0.946569 0.297245 11.00000 -1.20000 AFIX 0 C30 1 0.677772 0.858564 0.284692 11.00000 0.00836 0.02562 = 0.06018 0.00275 -0.00717 0.00707 C31 1 0.613007 0.815036 0.246958 11.00000 0.02593 0.03391 = 0.04104 0.00278 0.00078 -0.00403 AFIX 43 H31 2 0.539066 0.775270 0.252314 11.00000 -1.20000 AFIX 0 C32 1 0.658291 0.830751 0.201529 11.00000 0.01899 0.02706 = 0.06559 0.00243 -0.00724 0.01102 AFIX 43 H32 2 0.614185 0.800394 0.177391 11.00000 -1.20000 AFIX 0 C33 1 0.809968 0.910432 0.142437 11.00000 0.02076 0.01170 = 0.04459 0.00284 -0.01276 0.00263 AFIX 13 H33 2 0.790614 0.973545 0.135697 11.00000 -1.20000 AFIX 0 C34 1 0.958880 0.891012 0.133567 11.00000 0.03255 0.03363 = 0.05003 0.00100 -0.01501 -0.01252 AFIX 43 H34 2 0.986251 0.831223 0.133952 11.00000 -1.20000 AFIX 0 C35 1 1.059183 0.951670 0.124948 11.00000 0.05004 0.08704 = 0.07435 0.02488 -0.00740 -0.02873 AFIX 93 H35A 2 1.036384 1.012210 0.124242 11.00000 -1.20000 H35B 2 1.151876 0.933397 0.119649 11.00000 -1.20000 AFIX 0 C36 1 0.660496 0.895185 0.076306 11.00000 0.01311 0.01109 = 0.02604 0.00170 -0.00059 -0.00817 C37 1 0.503498 0.857590 0.012045 11.00000 0.03391 0.01077 = 0.04034 0.00923 -0.01274 -0.00409 AFIX 13 H37 2 0.546180 0.908302 -0.004341 11.00000 -1.20000 AFIX 0 C38 1 0.485369 0.781109 -0.021779 11.00000 0.08742 0.03040 = 0.05391 -0.01077 -0.03770 0.00041 AFIX 137 H38A 2 0.575684 0.765553 -0.034716 11.00000 -1.50000 H38B 2 0.422353 0.798998 -0.046167 11.00000 -1.50000 H38C 2 0.446565 0.730241 -0.005919 11.00000 -1.50000 AFIX 0 C39 1 0.364773 0.885421 0.030060 11.00000 0.06089 0.07446 = 0.06573 0.00534 -0.01679 0.00674 AFIX 137 H39A 2 0.320130 0.835631 0.045173 11.00000 -1.50000 H39B 2 0.306367 0.905506 0.004913 11.00000 -1.50000 H39C 2 0.377234 0.933302 0.051859 11.00000 -1.50000 AFIX 0 HKLF 4 REM cu_30926b in P2(1)2(1)2(1) REM R1 = 0.1024 for 6253 Fo > 4sig(Fo) and 0.1106 for all 6977 data REM 466 parameters refined using 72 restraints END WGHT 0.1037 46.4211 REM Highest difference peak 1.353, deepest hole -0.849, 1-sigma level 0.199 Q1 1 0.6755 0.8934 0.3498 11.00000 0.05 1.35 Q2 1 0.8597 0.8379 0.8488 11.00000 0.05 1.27 Q3 1 0.5834 0.9193 0.3490 11.00000 0.05 1.15 Q4 1 0.4979 0.0733 0.1114 11.00000 0.05 1.12 Q5 1 0.9379 0.7925 0.8518 11.00000 0.05 1.07 Q6 1 0.4522 -0.0273 0.1509 11.00000 0.05 1.03 Q7 1 0.4268 0.1127 0.1491 11.00000 0.05 1.01 Q8 1 0.3958 0.1063 0.1462 11.00000 0.05 1.01 Q9 1 0.3469 0.0071 0.1507 11.00000 0.05 0.98 Q10 1 0.3805 0.0953 0.1180 11.00000 0.05 0.96 ; _shelx_res_checksum 77003 _shelx_hkl_file ; 1 0 0 0.03 0.04 -1 0 0 0.21 0.05 3 0 0 0.20 0.13 4 0 0 18.29 1.59 -4 0 0 17.88 1.53 -7 0 0 0.46 0.35 -8 0 0 1.14 0.42 -9 0 0 0.59 0.37 -9 0 0 0.60 0.27 -10 0 0 0.54 0.31 -10 0 0 0.24 0.23 -11 0 0 0.10 0.17 0 -1 0 -0.03 0.02 0 -1 0 -0.04 0.03 1 1 0 -0.31 0.05 -1 -1 0 -0.26 0.05 -1 1 0 -0.27 0.05 1 -1 0 -0.22 0.05 -2 1 0 48.08 3.54 -2 -1 0 42.85 3.53 -3 -1 0 57.15 3.91 -3 1 0 50.30 3.87 3 1 0 41.36 4.10 3 -1 0 49.48 4.10 -4 1 0 76.26 5.87 -4 -1 0 72.97 5.89 4 -1 0 77.08 6.21 4 1 0 73.78 6.22 -5 1 0 32.20 2.84 5 1 0 37.94 3.03 6 1 0 36.13 3.15 -7 -1 0 6.73 0.84 -7 1 0 6.93 0.79 -8 1 0 3.83 0.57 -8 -1 0 3.73 0.66 -9 -1 0 3.65 0.64 -9 1 0 3.62 0.59 -9 1 0 4.06 0.50 -9 -1 0 4.08 0.53 -10 -1 0 2.11 0.43 -10 1 0 1.91 0.39 -10 -1 0 2.10 0.31 -10 1 0 1.93 0.29 -11 -1 0 1.66 0.28 -11 1 0 1.35 0.21 0 -2 0 43.20 2.97 0 -2 0 33.74 3.16 -1 2 0 -0.02 0.03 1 2 0 0.05 0.08 -1 -2 0 0.13 0.06 1 -2 0 0.07 0.09 2 -2 0 277.22 19.52 -2 2 0 238.41 18.35 2 2 0 202.63 19.51 -3 2 0 5.26 0.51 3 -2 0 5.75 0.55 3 2 0 4.40 0.54 4 -2 0 1.80 0.34 -4 2 0 2.07 0.32 4 2 0 1.97 0.34 5 2 0 4.25 0.54 -5 2 0 4.21 0.52 6 2 0 9.01 1.06 -6 -2 0 11.84 1.09 -7 -2 0 11.33 1.16 -7 2 0 10.37 1.07 -8 -2 0 1.96 0.52 -8 -2 0 1.79 0.33 -8 2 0 1.79 0.38 -9 -2 0 3.94 0.55 -9 2 0 3.93 0.47 -9 -2 0 3.58 0.59 -9 2 0 3.58 0.56 -10 2 0 3.96 0.46 -10 -2 0 4.35 0.63 -10 -2 0 4.33 0.51 -11 -2 0 1.03 0.22 0 -3 0 0.09 0.06 0 -3 0 0.11 0.09 1 3 0 188.29 15.57 1 -3 0 186.28 15.55 -1 3 0 197.79 14.63 2 3 0 105.20 9.46 -2 3 0 112.70 8.89 -2 -3 0 128.06 8.88 3 3 0 97.01 8.24 3 -3 0 93.95 8.24 -3 -3 0 105.63 7.74 -3 3 0 102.71 7.73 -4 3 0 4.56 0.52 4 3 0 5.52 0.60 5 3 0 13.06 1.16 -5 3 0 10.16 1.04 -6 -3 0 4.22 0.66 -7 -3 0 16.39 1.59 -7 3 0 15.63 1.48 -8 3 0 4.14 0.59 -8 3 0 4.06 0.50 -8 -3 0 4.65 0.61 -8 -3 0 4.58 0.76 -9 -3 0 1.73 0.37 -9 3 0 2.30 0.36 -9 3 0 2.12 0.38 -9 -3 0 1.68 0.50 -10 -3 0 2.88 0.52 -10 -3 0 2.85 0.43 -11 -3 0 0.28 0.18 0 -4 0 4.20 0.39 -1 -4 0 199.45 14.08 -1 4 0 177.16 14.09 1 4 0 173.94 14.99 2 -4 0 8.15 0.78 -3 4 0 1.62 0.27 -3 -4 0 1.87 0.26 3 4 0 1.47 0.30 4 4 0 12.45 1.18 -4 4 0 11.80 1.07 -5 4 0 44.17 4.12 5 4 0 60.56 4.48 -6 4 0 7.41 0.76 -7 -4 0 11.13 1.16 -7 4 0 9.34 0.99 -8 -4 0 10.05 0.90 -8 -4 0 8.69 0.86 -8 -4 0 7.14 1.05 9 4 0 1.12 0.60 -9 -4 0 1.01 0.47 -9 -4 0 0.33 0.32 -10 -4 0 0.98 0.41 -10 -4 0 0.58 0.26 -11 -4 0 0.21 0.17 0 5 0 0.13 0.13 1 -5 0 29.29 2.59 -1 5 0 31.27 2.44 1 5 0 30.21 2.62 -1 -5 0 32.43 2.43 2 5 0 11.02 1.04 -2 5 0 10.42 0.94 -2 -5 0 11.30 0.92 3 5 0 1.52 0.33 -3 5 0 1.72 0.28 -4 5 0 83.93 7.11 4 5 0 99.04 7.64 5 5 0 2.88 0.49 -5 5 0 2.51 0.39 -6 -5 0 7.40 0.93 7 5 0 2.10 0.71 -7 -5 0 0.23 0.51 -8 -5 0 2.25 0.33 -8 -5 0 2.08 0.40 -8 -5 0 2.25 0.60 9 5 0 -0.44 0.56 -9 -5 0 0.48 0.45 -9 -5 0 -0.16 0.31 -10 -5 0 0.56 0.26 0 6 0 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29 1.82 0.28 1 -1 29 2.14 0.39 -1 1 29 2.11 0.35 -1 1 29 2.14 0.36 -1 -1 29 2.03 0.38 1 1 29 1.95 0.36 -1 -1 29 2.01 0.36 1 1 29 2.14 0.35 -2 1 29 1.40 0.30 2 -1 29 1.23 0.33 -2 1 29 1.25 0.23 2 -1 29 0.92 0.22 2 1 29 1.58 0.33 2 1 29 1.17 0.22 3 -1 29 5.00 0.56 3 -1 29 6.00 0.66 3 1 29 5.34 0.55 3 1 29 6.78 0.64 4 -1 29 3.01 0.32 4 -1 -29 2.52 0.38 4 1 29 2.63 0.31 5 -1 29 1.24 0.18 5 -1 -29 0.79 0.21 6 -1 -29 0.18 0.15 0 -2 29 2.21 0.31 0 2 29 2.21 0.36 0 2 29 2.19 0.36 0 -2 29 2.60 0.42 -1 2 29 4.86 0.58 -1 2 29 4.25 0.52 1 -2 29 5.25 0.65 1 -2 29 4.16 0.53 1 2 29 5.08 0.52 1 2 29 4.88 0.60 -1 -2 29 5.18 0.53 -1 -2 29 5.70 0.65 -2 2 29 0.64 0.20 2 -2 29 0.67 0.29 -2 2 29 0.87 0.27 2 -2 29 0.56 0.20 2 2 29 0.69 0.26 2 2 29 0.38 0.19 3 -2 29 2.77 0.40 3 -2 29 2.24 0.33 3 -2 -29 1.77 0.41 3 -2 -29 1.78 0.31 3 2 29 2.38 0.30 4 -2 29 -0.20 0.13 4 -2 -29 0.17 0.19 5 -2 29 6.17 0.54 5 -2 -29 5.52 0.60 6 -2 -29 0.88 0.19 0 3 29 -0.06 0.18 0 3 29 0.18 0.24 0 -3 29 0.13 0.19 0 -3 29 0.17 0.29 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29 0.25 0.22 0 -5 -29 0.27 0.26 0 -5 29 0.16 0.20 0 5 29 0.09 0.17 1 -5 29 3.09 0.46 1 -5 29 1.99 0.38 -1 5 29 2.72 0.35 -1 5 29 3.36 0.40 1 5 29 2.57 0.35 1 -5 -29 2.12 0.37 1 -5 -29 1.78 0.47 1 5 29 3.68 0.44 2 -5 29 -0.06 0.28 -2 5 29 -0.12 0.16 2 -5 29 -0.18 0.17 -2 5 29 0.10 0.20 2 -5 -29 0.46 0.34 2 5 29 0.50 0.21 2 -5 -29 0.21 0.24 2 5 29 0.25 0.15 -3 5 29 5.98 0.50 3 -5 29 4.94 0.51 3 -5 -29 4.01 0.57 4 -5 29 1.15 0.19 4 -5 -29 1.16 0.25 5 -5 29 2.23 0.24 5 -5 -29 1.47 0.27 0 6 29 9.82 0.87 0 -6 -29 8.97 0.96 0 6 29 10.13 0.89 -1 6 29 1.13 0.24 -1 6 29 1.22 0.19 1 -6 29 0.87 0.22 1 -6 -29 1.26 0.41 1 6 29 1.22 0.20 1 -6 -29 0.92 0.28 2 -6 29 3.36 0.41 -2 6 29 4.15 0.39 2 -6 -29 2.68 0.47 2 6 29 3.39 0.38 3 -6 29 4.38 0.46 -3 6 29 4.98 0.45 3 -6 -29 3.72 0.52 4 -6 29 0.87 0.18 -4 6 29 1.47 0.21 4 -6 -29 0.98 0.24 0 -7 -29 0.30 0.24 0 7 29 0.04 0.15 -1 -7 -29 1.76 0.32 -1 7 29 2.33 0.29 1 7 29 1.92 0.29 1 -7 -29 1.53 0.32 -2 7 29 2.30 0.28 2 -7 29 2.00 0.32 2 -7 -29 1.28 0.30 3 -7 29 0.57 0.17 -3 7 29 0.93 0.16 3 -7 -29 0.48 0.22 4 -7 29 2.26 0.29 -4 7 29 2.61 0.28 4 -7 -29 2.18 0.35 0 8 29 0.97 0.18 0 -8 -29 0.55 0.24 -1 -8 -29 0.16 0.21 -1 8 29 0.03 0.14 1 -8 -29 0.10 0.21 1 8 29 0.05 0.14 -2 8 29 1.79 0.24 2 -8 29 1.77 0.29 -2 -8 -29 1.19 0.25 2 -8 -29 1.22 0.27 -3 8 29 0.38 0.13 3 -8 29 0.17 0.14 3 -8 -29 0.15 0.18 0 9 29 1.47 0.23 0 -9 -29 1.06 0.24 -1 9 29 0.27 0.13 -1 -9 -29 0.21 0.20 1 -9 -29 0.05 0.19 -2 9 29 8.28 0.67 2 -9 -29 6.59 0.73 0 0 30 45.58 3.82 0 0 30 44.45 3.73 1 0 30 0.47 0.20 -1 0 30 1.03 0.30 1 0 30 0.96 0.30 -1 0 30 0.50 0.20 -2 0 30 0.10 0.17 2 0 30 0.11 0.25 2 0 30 -0.26 0.17 3 0 30 4.66 0.52 3 0 30 3.25 0.41 4 0 30 0.20 0.12 5 0 -30 0.40 0.15 0 -1 30 3.73 0.56 0 1 30 3.64 0.43 0 -1 30 2.57 0.44 0 1 30 4.16 0.52 1 -1 30 6.43 0.69 -1 1 30 5.97 0.66 -1 1 30 5.10 0.60 1 -1 30 5.18 0.60 1 1 30 6.37 0.68 -1 -1 30 7.02 0.70 -1 -1 30 5.92 0.60 1 1 30 6.14 0.60 -2 1 30 0.49 0.24 2 -1 30 0.02 0.17 -2 1 30 0.09 0.17 2 -1 30 0.32 0.26 2 1 30 -0.29 0.17 2 1 30 0.19 0.24 3 -1 30 2.86 0.37 3 -1 30 4.24 0.49 3 1 30 2.90 0.36 4 -1 30 1.75 0.23 4 1 30 1.23 0.21 4 -1 -30 1.26 0.22 5 -1 -30 1.50 0.26 0 2 30 0.36 0.24 0 2 30 0.04 0.17 0 -2 30 0.23 0.27 1 -2 30 0.79 0.22 -1 2 30 1.23 0.29 1 -2 30 1.43 0.35 -1 2 30 0.99 0.21 -1 -2 30 1.09 0.22 1 2 30 1.17 0.21 1 2 30 1.47 0.31 -2 2 30 12.51 1.10 -2 2 30 12.40 1.09 2 -2 30 12.50 1.10 2 -2 30 13.35 1.15 2 2 30 11.44 1.09 2 2 30 12.15 1.12 3 -2 30 1.14 0.20 3 -2 30 1.64 0.32 3 2 30 0.98 0.18 3 -2 -30 1.16 0.23 4 -2 30 0.47 0.14 4 -2 -30 0.57 0.19 5 -2 30 0.59 0.12 5 -2 -30 0.35 0.16 0 -3 30 0.09 0.19 0 -3 30 0.59 0.29 0 3 30 0.29 0.17 0 3 30 0.40 0.23 -1 3 30 7.28 0.72 1 -3 30 7.30 0.73 -1 3 30 7.62 0.75 1 -3 30 8.57 0.83 1 3 30 7.62 0.77 1 3 30 7.88 0.72 -2 3 30 9.78 0.89 -2 3 30 9.93 0.88 2 -3 30 9.99 0.96 2 -3 30 8.76 0.89 2 3 30 9.61 0.88 2 3 30 10.76 0.92 -3 3 30 3.51 0.35 3 -3 30 2.92 0.35 3 -3 -30 2.47 0.40 3 3 30 2.72 0.33 4 -3 30 0.72 0.15 4 -3 -30 0.38 0.19 5 -3 30 1.89 0.21 5 -3 -30 1.14 0.23 0 4 30 0.41 0.17 0 -4 30 0.01 0.18 0 4 30 0.48 0.22 0 -4 30 0.80 0.29 1 -4 30 9.75 0.92 -1 4 30 9.49 0.92 -1 4 30 9.91 0.91 1 -4 30 11.24 1.01 1 4 30 10.37 0.91 1 4 30 10.33 0.94 -2 4 30 2.72 0.32 -2 4 30 2.63 0.37 2 -4 30 2.41 0.40 2 -4 30 1.98 0.33 2 -4 -30 2.29 0.39 2 4 30 2.12 0.31 3 -4 30 -0.01 0.15 -3 4 30 0.26 0.14 3 -4 -30 0.28 0.20 3 4 30 0.09 0.12 4 -4 30 0.40 0.13 4 -4 -30 0.29 0.19 5 -4 -30 2.13 0.31 0 5 30 0.49 0.21 0 5 30 0.32 0.16 -1 5 30 2.20 0.35 -1 5 30 2.25 0.30 1 -5 30 2.11 0.33 1 -5 -30 1.54 0.31 1 5 30 2.22 0.31 -2 5 30 2.55 0.29 2 -5 30 1.83 0.31 2 5 30 1.87 0.29 2 -5 -30 1.60 0.30 -3 5 30 0.04 0.13 3 -5 30 -0.20 0.14 3 -5 -30 -0.07 0.19 4 -5 30 4.74 0.43 4 -5 -30 3.83 0.48 0 -6 -30 0.19 0.21 0 6 30 0.24 0.15 1 -6 30 10.09 0.86 -1 6 30 9.73 0.84 1 -6 -30 7.67 0.90 1 6 30 9.71 0.84 -2 6 30 0.81 0.16 2 -6 30 0.55 0.17 2 -6 -30 0.69 0.23 2 6 30 0.80 0.16 3 -6 30 0.63 0.16 -3 6 30 0.85 0.15 3 -6 -30 0.70 0.21 4 -6 30 0.60 0.14 4 -6 -30 0.52 0.18 0 7 30 3.09 0.34 0 -7 -30 2.69 0.42 1 -7 30 0.73 0.18 -1 -7 -30 0.56 0.21 -1 7 30 0.58 0.15 1 -7 -30 0.46 0.22 1 7 30 0.57 0.15 2 -7 30 2.19 0.30 -2 7 30 1.94 0.26 2 -7 -30 1.46 0.28 3 -7 30 2.26 0.29 -3 7 30 2.30 0.27 3 -7 -30 1.94 0.33 0 8 30 0.42 0.13 0 -8 -30 0.40 0.19 -1 -8 -30 0.23 0.17 -1 8 30 0.23 0.12 1 8 30 0.42 0.13 1 -8 -30 0.28 0.18 -2 8 30 1.57 0.23 2 -8 -30 1.72 0.30 0 0 31 -0.01 0.24 -1 0 31 10.36 0.98 -1 0 31 11.09 1.02 1 0 31 10.82 0.98 1 0 31 11.44 1.02 2 0 31 1.46 0.30 2 0 31 1.11 0.21 -2 0 31 1.15 0.20 4 0 31 1.59 0.22 0 1 31 5.58 0.64 0 -1 31 5.83 0.59 0 -1 31 6.85 0.68 0 1 31 5.56 0.58 -1 1 31 3.72 0.47 1 -1 31 3.33 0.50 1 -1 31 2.90 0.39 -1 1 31 3.05 0.39 -1 -1 31 4.18 0.51 1 1 31 2.90 0.39 1 1 31 3.96 0.49 -1 -1 31 2.70 0.39 2 -1 31 3.48 0.49 -2 1 31 3.27 0.37 2 -1 31 3.02 0.38 2 1 31 2.82 0.36 3 -1 31 0.76 0.16 3 1 31 0.67 0.16 4 -1 31 1.22 0.21 4 1 31 1.36 0.20 0 -2 31 0.75 0.20 0 2 31 0.77 0.24 0 2 31 0.79 0.19 0 -2 31 1.31 0.31 -1 2 31 1.88 0.30 -1 2 31 1.84 0.30 1 -2 31 2.02 0.36 1 -2 31 1.59 0.25 1 2 31 1.69 0.24 -1 -2 31 1.80 0.31 1 2 31 1.96 0.33 2 -2 31 0.06 0.15 -2 2 31 0.31 0.15 2 2 31 0.13 0.15 3 -2 31 0.43 0.16 3 2 31 0.68 0.15 4 -2 31 5.56 0.46 4 -2 -31 3.84 0.48 0 -3 31 4.84 0.52 0 3 31 5.09 0.56 0 3 31 5.08 0.51 1 -3 31 0.79 0.19 -1 3 31 1.10 0.18 -1 3 31 1.01 0.25 1 3 31 0.87 0.19 -2 3 31 8.64 0.77 2 -3 31 8.22 0.78 2 3 31 8.64 0.77 3 -3 31 0.95 0.18 -3 3 31 1.28 0.23 3 -3 -31 1.12 0.22 3 3 31 1.49 0.22 4 -3 31 0.30 0.12 4 -3 -31 0.29 0.15 0 -4 31 4.52 0.47 0 4 31 4.31 0.45 -1 4 31 0.71 0.16 1 -4 31 0.52 0.17 1 4 31 0.48 0.16 2 -4 31 4.65 0.46 -2 4 31 4.49 0.44 2 -4 -31 3.76 0.48 2 4 31 4.52 0.44 3 -4 31 0.80 0.17 -3 4 31 1.11 0.16 3 -4 -31 0.82 0.20 4 -4 31 0.94 0.16 4 -4 -31 0.92 0.19 0 5 31 0.61 0.15 1 -5 31 0.30 0.15 -1 5 31 0.14 0.13 1 -5 -31 0.31 0.18 1 5 31 0.17 0.14 -2 5 31 1.30 0.24 2 -5 31 1.43 0.21 2 -5 -31 1.34 0.25 2 5 31 1.74 0.24 3 -5 31 0.14 0.13 -3 5 31 0.33 0.12 3 -5 -31 0.40 0.17 4 -5 31 1.24 0.21 0 6 31 7.35 0.67 1 -6 31 2.68 0.32 -1 6 31 2.26 0.30 1 6 31 2.73 0.30 1 -6 -31 2.20 0.36 2 -6 31 2.24 0.31 -2 6 31 2.31 0.28 2 6 31 2.42 0.28 2 -6 -31 1.91 0.33 -3 6 31 0.44 0.12 3 -6 31 0.39 0.13 3 -6 -31 0.37 0.16 0 7 31 1.29 0.21 0 -7 -31 0.98 0.22 -1 7 31 -0.07 0.11 1 7 31 0.27 0.12 1 -7 -31 0.23 0.17 2 -7 31 0.67 0.15 -2 7 31 0.49 0.13 2 -7 -31 0.77 0.19 -1 8 31 0.48 0.12 -1 0 32 2.22 0.31 1 0 32 2.06 0.30 2 0 32 0.70 0.16 3 0 32 0.48 0.13 1 -1 32 -0.16 0.14 -1 1 32 0.10 0.14 -1 -1 32 -0.18 0.14 1 1 32 -0.17 0.14 2 -1 32 3.46 0.40 -2 1 32 3.73 0.40 2 1 32 4.09 0.40 3 -1 32 1.70 0.24 3 1 32 1.55 0.24 4 -1 32 0.10 0.10 0 -2 32 4.25 0.43 0 2 32 3.71 0.42 1 -2 32 0.27 0.15 -1 2 32 0.44 0.14 -1 -2 32 0.40 0.15 1 2 32 0.21 0.15 -2 2 32 0.14 0.13 2 -2 32 -0.03 0.14 2 2 32 0.08 0.13 3 -2 32 4.41 0.45 3 2 32 4.67 0.44 4 -2 32 1.63 0.22 0 3 32 0.63 0.16 0 -3 32 0.87 0.17 -1 3 32 3.80 0.38 1 -3 32 3.83 0.40 1 3 32 3.39 0.39 2 -3 32 -0.13 0.13 -2 3 32 0.06 0.12 2 3 32 0.02 0.12 3 -3 32 3.21 0.36 3 3 32 3.45 0.34 0 4 32 0.78 0.15 0 -4 32 0.89 0.17 -1 4 32 1.61 0.25 1 -4 32 1.90 0.27 1 4 32 1.62 0.26 2 -4 32 0.90 0.17 -2 4 32 0.91 0.15 2 4 32 1.19 0.20 -3 4 32 -0.06 0.10 0 5 32 -0.17 0.11 -1 5 32 0.34 0.12 1 -5 32 0.55 0.14 1 5 32 0.67 0.14 -2 5 32 -0.03 0.11 2 -5 32 -0.20 0.12 2 -5 -32 0.22 0.14 2 5 32 0.20 0.11 3 -5 32 1.26 0.21 0 6 32 4.31 0.42 -1 6 32 0.63 0.13 1 6 32 0.81 0.14 2 -6 32 1.17 0.21 -2 6 32 1.02 0.14 0 0 33 -0.10 0.12 1 0 33 0.05 0.13 -1 0 33 0.15 0.13 2 0 33 6.50 0.60 3 0 33 1.25 0.20 0 1 33 0.27 0.13 0 -1 33 0.27 0.13 1 -1 33 4.86 0.50 -1 1 33 5.36 0.49 -1 -1 33 5.46 0.50 1 1 33 4.99 0.49 2 -1 33 0.43 0.14 -2 1 33 0.73 0.14 2 1 33 0.81 0.15 3 -1 33 0.57 0.12 3 1 33 0.62 0.13 0 -2 33 5.75 0.51 0 2 33 4.87 0.50 1 -2 33 1.33 0.24 -1 2 33 1.54 0.23 1 2 33 1.24 0.23 -2 2 33 0.03 0.11 2 -2 33 -0.25 0.11 2 2 33 -0.04 0.11 3 -2 33 1.79 0.24 0 -3 33 4.07 0.40 0 3 33 3.62 0.38 -1 3 33 7.44 0.67 1 -3 33 8.11 0.69 1 3 33 7.09 0.67 2 -3 33 0.21 0.12 -2 3 33 0.34 0.11 2 3 33 0.52 0.12 3 -3 33 -0.06 0.10 0 4 33 0.52 0.13 1 -4 33 0.77 0.14 -1 4 33 0.78 0.13 1 4 33 0.81 0.14 2 -4 33 0.39 0.12 -2 4 33 0.50 0.11 0 5 33 0.26 0.11 -1 5 33 0.21 0.10 1 5 33 0.33 0.11 0 0 34 8.40 0.75 1 0 34 2.33 0.28 -1 0 34 2.52 0.28 2 0 34 1.34 0.20 0 -1 34 0.16 0.11 0 1 34 0.20 0.11 -1 1 34 3.56 0.34 1 -1 34 3.15 0.35 1 1 34 3.45 0.35 2 -1 34 1.41 0.21 2 1 34 1.30 0.20 0 2 34 0.23 0.11 0 -2 34 0.15 0.11 -1 2 34 0.99 0.18 1 -2 34 0.73 0.15 1 2 34 1.12 0.19 2 -2 34 3.21 0.33 0 3 34 2.63 0.28 -1 3 34 1.90 0.24 1 -3 34 2.33 0.25 1 3 34 2.05 0.24 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 9948 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Br1 Br 0.4315(2) 0.04817(15) 0.15032(7) 0.0558(6) Uani 1 1 d . . N1 N 0.3975(12) 0.0064(8) 0.4395(4) 0.024(3) Uani 1 1 d . . H1 H 0.3729 -0.0480 0.4343 0.029 Uiso 1 1 calc R U O1 O 0.2632(11) 0.0395(6) 0.3786(3) 0.025(2) Uani 1 1 d . U O2 O 0.3675(14) 0.1522(7) 0.4184(4) 0.041(3) Uani 1 1 d . U C1 C 0.2490(15) 0.0891(9) 0.2998(5) 0.022(3) Uani 1 1 d . . C2 C 0.177(2) 0.1183(12) 0.2616(5) 0.042(4) Uani 1 1 d . . H2 H 0.0898 0.1455 0.2658 0.051 Uiso 1 1 calc R U C3 C 0.2292(17) 0.1092(12) 0.2171(6) 0.038(4) Uani 1 1 d . . H3 H 0.1788 0.1328 0.1923 0.045 Uiso 1 1 calc R U C4 C 0.3576(14) 0.0646(10) 0.2092(6) 0.030(3) Uani 1 1 d . . C5 C 0.4324(16) 0.0346(11) 0.2478(5) 0.031(3) Uani 1 1 d . . H5 H 0.5186 0.0057 0.2437 0.037 Uiso 1 1 calc R U C6 C 0.3819(19) 0.0469(11) 0.2916(5) 0.037(4) Uani 1 1 d . . H6 H 0.4353 0.0272 0.3166 0.044 Uiso 1 1 calc R U C7 C 0.1913(17) 0.1018(9) 0.3482(5) 0.029(3) Uani 1 1 d . . H7 H 0.2188 0.1621 0.3581 0.035 Uiso 1 1 calc R U C8 C 0.0342(16) 0.0961(11) 0.3529(6) 0.034(3) Uani 1 1 d . U H8 H -0.0212 0.1368 0.3366 0.041 Uiso 1 1 calc R U C9 C -0.0292(18) 0.0370(15) 0.3786(7) 0.052(5) Uani 1 1 d . . H9A H 0.0238 -0.0045 0.3953 0.062 Uiso 1 1 calc R U H9B H -0.1274 0.0362 0.3804 0.062 Uiso 1 1 calc R U C10 C 0.3420(16) 0.0735(8) 0.4136(4) 0.021(3) Uani 1 1 d . . C11 C 0.4982(16) 0.0260(10) 0.4761(5) 0.027(3) Uani 1 1 d . . H11 H 0.4641 0.0780 0.4935 0.032 Uiso 1 1 calc R U C12 C 0.509(2) -0.0523(13) 0.5086(7) 0.054(5) Uani 1 1 d . . H12A H 0.4195 -0.0620 0.5233 0.081 Uiso 1 1 calc R U H12B H 0.5799 -0.0402 0.5316 0.081 Uiso 1 1 calc R U H12C H 0.5354 -0.1049 0.4914 0.081 Uiso 1 1 calc R U C13 C 0.646(2) 0.0476(14) 0.4569(7) 0.053(5) Uani 1 1 d . . H13A H 0.6758 0.0000 0.4368 0.080 Uiso 1 1 calc R U H13B H 0.7113 0.0535 0.4820 0.080 Uiso 1 1 calc R U H13C H 0.6419 0.1026 0.4398 0.080 Uiso 1 1 calc R U Br2 Br 0.8120(2) 0.77103(16) 0.85462(7) 0.0586(6) Uani 1 1 d . . N2 N 0.8755(13) 0.8291(8) 0.5569(4) 0.025(3) Uani 1 1 d . U H2A H 0.8506 0.8832 0.5629 0.030 Uiso 1 1 calc R U O3 O 0.7484(12) 0.7927(6) 0.6196(3) 0.028(2) Uani 1 1 d . . O4 O 0.8457(12) 0.6820(7) 0.5745(3) 0.032(2) Uani 1 1 d . U C14 C 0.7087(15) 0.7390(9) 0.6980(5) 0.024(3) Uani 1 1 d . . C15 C 0.705(2) 0.6643(11) 0.7270(6) 0.038(4) Uani 1 1 d . . H15 H 0.6814 0.6083 0.7152 0.046 Uiso 1 1 calc R U C16 C 0.737(2) 0.6746(11) 0.7738(6) 0.045(4) Uani 1 1 d . . H16 H 0.7385 0.6246 0.7929 0.054 Uiso 1 1 calc R U C17 C 0.7661(17) 0.7591(11) 0.7924(5) 0.035(4) Uani 1 1 d . . C18 C 0.7690(19) 0.8311(12) 0.7626(6) 0.040(4) Uani 1 1 d . . H18 H 0.7938 0.8871 0.7741 0.048 Uiso 1 1 calc R U C19 C 0.736(2) 0.8227(10) 0.7160(6) 0.041(4) Uani 1 1 d . . H19 H 0.7322 0.8730 0.6971 0.049 Uiso 1 1 calc R U C20 C 0.6736(16) 0.7252(9) 0.6466(5) 0.030(3) Uani 1 1 d . . H20 H 0.7046 0.6654 0.6369 0.037 Uiso 1 1 calc R U C21 C 0.5217(15) 0.7347(11) 0.6381(5) 0.032(3) Uani 1 1 d . . H21 H 0.4627 0.6992 0.6562 0.038 Uiso 1 1 calc R U C22 C 0.459(2) 0.7866(15) 0.6082(6) 0.052(5) Uani 1 1 d . . H22A H 0.5121 0.8237 0.5891 0.063 Uiso 1 1 calc R U H22B H 0.3606 0.7866 0.6061 0.063 Uiso 1 1 calc R U C23 C 0.8270(13) 0.7615(8) 0.5826(4) 0.016(2) Uani 1 1 d . U C24 C 0.9722(17) 0.8099(10) 0.5184(5) 0.027(3) Uani 1 1 d . . H24 H 0.9441 0.7534 0.5038 0.033 Uiso 1 1 calc R U C25 C 1.1269(17) 0.8015(14) 0.5359(7) 0.048(5) Uani 1 1 d . . H25A H 1.1585 0.8584 0.5473 0.072 Uiso 1 1 calc R U H25B H 1.1868 0.7829 0.5108 0.072 Uiso 1 1 calc R U H25C H 1.1312 0.7580 0.5603 0.072 Uiso 1 1 calc R U C26 C 0.959(3) 0.8848(12) 0.4832(6) 0.060(6) Uani 1 1 d . . H26A H 0.8672 0.8827 0.4691 0.089 Uiso 1 1 calc R U H26B H 1.0304 0.8777 0.4598 0.089 Uiso 1 1 calc R U H26C H 0.9715 0.9414 0.4984 0.089 Uiso 1 1 calc R U Br3 Br 0.6171(2) 0.84274(17) 0.34440(8) 0.0607(6) Uani 1 1 d . . N3 N 0.5943(13) 0.8331(8) 0.0500(4) 0.026(3) Uani 1 1 d . U H3A H 0.6068 0.7773 0.0562 0.031 Uiso 1 1 calc R U O5 O 0.7291(11) 0.8545(7) 0.1116(4) 0.030(2) Uani 1 1 d . U O6 O 0.6555(11) 0.9756(6) 0.0704(4) 0.028(2) Uani 1 1 d . U C27 C 0.7649(17) 0.8891(10) 0.1915(5) 0.029(3) Uani 1 1 d . U C28 C 0.8368(16) 0.9288(10) 0.2277(6) 0.032(3) Uani 1 1 d . . H28 H 0.9151 0.9645 0.2213 0.038 Uiso 1 1 calc R U C29 C 0.7953(15) 0.9169(10) 0.2737(6) 0.030(3) Uani 1 1 d . . H29 H 0.8433 0.9466 0.2972 0.036 Uiso 1 1 calc R U C30 C 0.6778(14) 0.8586(10) 0.2847(6) 0.031(3) Uani 1 1 d . . C31 C 0.6130(18) 0.8150(11) 0.2470(5) 0.034(3) Uani 1 1 d . U H31 H 0.5391 0.7753 0.2523 0.040 Uiso 1 1 calc R U C32 C 0.6583(16) 0.8308(11) 0.2015(6) 0.037(4) Uani 1 1 d . . H32 H 0.6142 0.8004 0.1774 0.045 Uiso 1 1 calc R U C33 C 0.8100(15) 0.9104(9) 0.1424(5) 0.026(3) Uani 1 1 d . . H33 H 0.7906 0.9735 0.1357 0.031 Uiso 1 1 calc R U C34 C 0.9589(18) 0.8910(12) 0.1336(6) 0.039(4) Uani 1 1 d . . H34 H 0.9863 0.8312 0.1340 0.046 Uiso 1 1 calc R U C35 C 1.059(3) 0.9517(19) 0.1249(8) 0.070(7) Uani 1 1 d . . H35A H 1.0364 1.0122 0.1242 0.085 Uiso 1 1 calc R U H35B H 1.1519 0.9334 0.1196 0.085 Uiso 1 1 calc R U C36 C 0.6605(13) 0.8952(8) 0.0763(4) 0.017(3) Uani 1 1 d . U C37 C 0.5035(16) 0.8576(9) 0.0120(5) 0.028(3) Uani 1 1 d . . H37 H 0.5462 0.9083 -0.0043 0.034 Uiso 1 1 calc R U C38 C 0.485(3) 0.7811(13) -0.0218(7) 0.057(6) Uani 1 1 d . . H38A H 0.5757 0.7656 -0.0347 0.086 Uiso 1 1 calc R U H38B H 0.4224 0.7990 -0.0462 0.086 Uiso 1 1 calc R U H38C H 0.4466 0.7302 -0.0059 0.086 Uiso 1 1 calc R U C39 C 0.365(3) 0.8854(17) 0.0301(8) 0.067(6) Uani 1 1 d . . H39A H 0.3201 0.8356 0.0452 0.101 Uiso 1 1 calc R U H39B H 0.3064 0.9055 0.0049 0.101 Uiso 1 1 calc R U H39C H 0.3772 0.9333 0.0519 0.101 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 0.0626(13) 0.0614(13) 0.0435(10) -0.0039(9) 0.0129(10) -0.0077(10) N1 0.018(6) 0.011(6) 0.042(7) -0.002(4) -0.009(5) -0.001(4) O1 0.031(4) 0.014(4) 0.030(4) 0.005(3) -0.013(4) -0.002(3) O2 0.064(7) 0.007(5) 0.050(6) 0.001(4) -0.019(5) -0.002(5) C1 0.018(6) 0.019(7) 0.029(7) 0.004(5) -0.002(5) -0.003(5) C2 0.054(11) 0.039(10) 0.034(8) 0.000(7) -0.012(8) 0.026(8) C3 0.025(8) 0.054(11) 0.034(8) 0.011(7) -0.005(6) 0.005(7) C4 0.014(7) 0.023(8) 0.053(9) 0.007(6) -0.003(6) -0.005(6) C5 0.015(7) 0.035(9) 0.042(8) 0.008(7) 0.008(6) 0.009(6) C6 0.039(9) 0.034(9) 0.037(8) 0.004(7) -0.005(7) 0.012(7) C7 0.043(8) 0.015(7) 0.029(7) 0.003(5) -0.007(7) 0.013(6) C8 0.028(5) 0.035(6) 0.039(6) 0.006(5) 0.001(5) 0.013(5) C9 0.017(8) 0.078(15) 0.062(12) -0.002(10) -0.007(8) -0.005(8) C10 0.033(8) 0.005(7) 0.024(6) -0.001(4) -0.003(5) 0.003(5) C11 0.020(7) 0.026(8) 0.035(8) -0.010(6) -0.007(6) -0.001(6) C12 0.072(14) 0.035(11) 0.054(11) 0.013(8) -0.032(10) -0.014(9) C13 0.046(12) 0.045(12) 0.069(12) 0.018(9) 0.003(9) -0.005(9) Br2 0.0591(12) 0.0770(15) 0.0398(9) -0.0087(10) -0.0080(9) 0.0219(11) N2 0.029(5) 0.018(5) 0.029(5) 0.001(4) 0.005(4) 0.006(4) O3 0.036(6) 0.008(5) 0.040(5) -0.004(4) 0.017(5) -0.003(4) O4 0.043(5) 0.018(4) 0.034(4) 0.001(3) 0.010(4) 0.009(3) C14 0.023(7) 0.012(7) 0.038(7) 0.002(5) 0.007(6) -0.005(5) C15 0.056(11) 0.018(8) 0.041(8) -0.003(6) -0.007(8) 0.007(7) C16 0.069(13) 0.027(10) 0.039(9) 0.006(7) 0.013(8) 0.008(8) C17 0.028(8) 0.038(10) 0.038(8) -0.002(7) 0.001(6) 0.013(7) C18 0.045(10) 0.031(9) 0.044(9) -0.010(7) 0.004(7) -0.014(8) C19 0.069(13) 0.008(8) 0.046(9) -0.001(6) 0.015(9) -0.009(7) C20 0.043(8) 0.014(7) 0.035(7) 0.000(6) 0.011(7) -0.012(6) C21 0.021(7) 0.031(8) 0.043(8) -0.004(7) -0.002(6) -0.010(6) C22 0.042(11) 0.067(14) 0.047(10) 0.005(9) -0.005(8) -0.012(10) C23 0.018(5) 0.005(5) 0.024(5) 0.000(4) 0.004(4) 0.004(4) C24 0.035(9) 0.019(8) 0.027(7) -0.003(5) 0.008(6) 0.012(6) C25 0.013(7) 0.074(14) 0.058(11) -0.003(9) -0.005(7) 0.006(8) C26 0.12(2) 0.023(10) 0.039(9) 0.008(7) 0.017(11) 0.008(10) Br3 0.0579(12) 0.0728(15) 0.0515(12) 0.0151(10) 0.0078(10) 0.0142(11) N3 0.029(5) 0.012(5) 0.037(5) 0.004(4) -0.009(4) 0.001(4) O5 0.033(4) 0.015(4) 0.040(4) 0.002(4) -0.009(4) -0.002(4) O6 0.033(5) 0.009(5) 0.041(5) 0.003(4) -0.007(4) 0.002(4) C27 0.034(6) 0.021(5) 0.031(5) 0.002(4) -0.005(5) -0.001(5) C28 0.019(7) 0.024(8) 0.053(9) 0.008(6) -0.016(6) -0.003(6) C29 0.016(7) 0.027(8) 0.049(9) -0.003(6) -0.006(6) -0.002(6) C30 0.008(6) 0.026(8) 0.060(10) 0.003(7) -0.007(6) 0.007(5) C31 0.026(6) 0.034(6) 0.041(6) 0.003(5) 0.001(5) -0.004(5) C32 0.019(7) 0.027(9) 0.066(11) 0.002(7) -0.007(7) 0.011(6) C33 0.021(6) 0.012(7) 0.045(8) 0.003(5) -0.013(6) 0.003(5) C34 0.033(9) 0.034(10) 0.050(10) 0.001(7) -0.015(7) -0.013(7) C35 0.050(13) 0.087(18) 0.074(14) 0.025(13) -0.007(11) -0.029(13) C36 0.013(5) 0.011(5) 0.026(5) 0.002(4) -0.001(4) -0.008(4) C37 0.034(8) 0.011(7) 0.040(8) 0.009(6) -0.013(6) -0.004(6) C38 0.087(16) 0.030(11) 0.054(11) -0.011(8) -0.038(11) 0.000(10) C39 0.061(14) 0.074(16) 0.066(14) 0.005(11) -0.017(11) 0.007(12) 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 C10 N1 C11 120.4(11) C10 O1 C7 117.9(11) C2 C1 C6 116.4(14) C2 C1 C7 121.8(14) C6 C1 C7 121.8(12) C1 C2 C3 122.9(16) C2 C3 C4 120.3(15) C5 C4 C3 117.5(15) C5 C4 Br1 120.0(11) C3 C4 Br1 122.5(12) C6 C5 C4 121.4(14) C5 C6 C1 121.5(14) O1 C7 C8 112.0(13) O1 C7 C1 108.1(11) C8 C7 C1 115.8(13) C9 C8 C7 123.3(15) O2 C10 O1 124.1(12) O2 C10 N1 125.3(13) O1 C10 N1 110.3(11) N1 C11 C12 110.0(13) N1 C11 C13 112.0(14) C12 C11 C13 109.0(15) C23 N2 C24 119.1(11) C23 O3 C20 116.2(10) C19 C14 C15 120.2(14) C19 C14 C20 121.9(13) C15 C14 C20 117.8(13) C16 C15 C14 119.2(15) C15 C16 C17 121.0(15) C18 C17 C16 117.9(15) C18 C17 Br2 121.6(13) C16 C17 Br2 120.3(12) C17 C18 C19 122.0(15) C14 C19 C18 119.4(15) O3 C20 C21 108.6(13) O3 C20 C14 108.6(11) C21 C20 C14 111.2(12) C22 C21 C20 128.1(16) O4 C23 N2 125.5(12) O4 C23 O3 123.5(11) N2 C23 O3 111.0(10) N2 C24 C26 108.2(13) N2 C24 C25 110.8(13) C26 C24 C25 110.8(17) C36 N3 C37 121.9(11) C36 O5 C33 117.4(10) C32 C27 C28 118.5(15) C32 C27 C33 122.8(14) C28 C27 C33 118.6(14) C27 C28 C29 121.8(14) C28 C29 C30 120.1(14) C31 C30 C29 116.2(15) C31 C30 Br3 122.2(12) C29 C30 Br3 121.7(12) C32 C31 C30 121.0(15) C27 C32 C31 122.2(16) O5 C33 C34 106.8(12) O5 C33 C27 107.8(12) C34 C33 C27 113.2(13) C35 C34 C33 126(2) O6 C36 N3 125.6(12) O6 C36 O5 124.7(12) N3 C36 O5 109.7(11) N3 C37 C39 109.5(14) N3 C37 C38 111.5(13) C39 C37 C38 109.9(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C4 1.854(16) N1 C10 1.356(17) N1 C11 1.451(17) O1 C10 1.354(16) O1 C7 1.448(15) O2 C10 1.208(17) C1 C2 1.36(2) C1 C6 1.42(2) C1 C7 1.51(2) C2 C3 1.38(2) C3 C4 1.40(2) C4 C5 1.39(2) C5 C6 1.36(2) C7 C8 1.49(2) C8 C9 1.30(3) C11 C12 1.50(2) C11 C13 1.53(2) Br2 C17 1.856(16) N2 C23 1.334(17) N2 C24 1.468(17) O3 C23 1.381(15) O3 C20 1.458(16) O4 C23 1.222(16) C14 C19 1.38(2) C14 C15 1.40(2) C14 C20 1.53(2) C15 C16 1.39(2) C16 C17 1.40(2) C17 C18 1.38(2) C18 C19 1.39(2) C20 C21 1.46(2) C21 C22 1.30(3) C24 C26 1.52(2) C24 C25 1.55(2) Br3 C30 1.832(17) N3 C36 1.352(17) N3 C37 1.440(17) O5 C36 1.352(16) O5 C33 1.440(16) O6 C36 1.214(16) C27 C32 1.36(2) C27 C28 1.38(2) C27 C33 1.51(2) C28 C29 1.39(2) C29 C30 1.45(2) C30 C31 1.41(2) C31 C32 1.40(2) C33 C34 1.46(2) C34 C35 1.33(3) C37 C39 1.47(3) C37 C38 1.51(2) 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 N1 H1 O4 0.86 2.03 2.887(15) 170.9 4_456 N2 H2A O6 0.86 2.12 2.959(15) 164.4 2_675 N3 H3A O2 0.86 2.02 2.875(15) 170.6 3_655 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 C6 C1 C2 C3 -1(3) C7 C1 C2 C3 178.6(16) C1 C2 C3 C4 3(3) C2 C3 C4 C5 -3(3) C2 C3 C4 Br1 178.8(14) C3 C4 C5 C6 1(2) Br1 C4 C5 C6 179.0(13) C4 C5 C6 C1 1(3) C2 C1 C6 C5 -1(2) C7 C1 C6 C5 179.1(15) C10 O1 C7 C8 -113.3(14) C10 O1 C7 C1 118.0(13) C2 C1 C7 O1 160.9(15) C6 C1 C7 O1 -19.7(19) C2 C1 C7 C8 34(2) C6 C1 C7 C8 -146.2(15) O1 C7 C8 C9 -5(2) C1 C7 C8 C9 119.5(19) C7 O1 C10 O2 -8(2) C7 O1 C10 N1 177.8(12) C11 N1 C10 O2 -1(2) C11 N1 C10 O1 173.3(12) C10 N1 C11 C12 162.5(15) C10 N1 C11 C13 -76.0(18) C19 C14 C15 C16 -4(3) C20 C14 C15 C16 179.8(16) C14 C15 C16 C17 3(3) C15 C16 C17 C18 -3(3) C15 C16 C17 Br2 -178.7(15) C16 C17 C18 C19 4(3) Br2 C17 C18 C19 179.5(14) C15 C14 C19 C18 4(3) C20 C14 C19 C18 -179.1(15) C17 C18 C19 C14 -5(3) C23 O3 C20 C21 -109.9(14) C23 O3 C20 C14 129.1(12) C19 C14 C20 O3 32(2) C15 C14 C20 O3 -151.7(14) C19 C14 C20 C21 -87.7(18) C15 C14 C20 C21 88.9(17) O3 C20 C21 C22 7(2) C14 C20 C21 C22 126.2(19) C24 N2 C23 O4 -7(2) C24 N2 C23 O3 174.5(12) C20 O3 C23 O4 -7(2) C20 O3 C23 N2 172.0(12) C23 N2 C24 C26 154.7(15) C23 N2 C24 C25 -83.6(17) C32 C27 C28 C29 -6(2) C33 C27 C28 C29 175.7(13) C27 C28 C29 C30 3(2) C28 C29 C30 C31 1(2) C28 C29 C30 Br3 -178.7(11) C29 C30 C31 C32 -2(2) Br3 C30 C31 C32 177.7(12) C28 C27 C32 C31 5(2) C33 C27 C32 C31 -176.7(14) C30 C31 C32 C27 -1(2) C36 O5 C33 C34 -109.7(14) C36 O5 C33 C27 128.4(12) C32 C27 C33 O5 -4.1(19) C28 C27 C33 O5 174.4(13) C32 C27 C33 C34 -122.0(16) C28 C27 C33 C34 56.5(19) O5 C33 C34 C35 128.8(18) C27 C33 C34 C35 -113(2) C37 N3 C36 O6 -3(2) C37 N3 C36 O5 174.9(12) C33 O5 C36 O6 -5(2) C33 O5 C36 N3 177.9(11) C36 N3 C37 C39 -78.7(19) C36 N3 C37 C38 159.4(15) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139184434