#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:45:10 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225901 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515776.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_4515776 loop_ _publ_author_name 'Struble, Thomas J.' 'Lankswert, Hannah M.' 'Pink, Maren' 'Johnston, Jeffrey N.' _publ_section_title ; Enantioselective Organocatalytic Amine-Isocyanate Capture-Cyclization: Regioselective Alkene Iodoamination for the Synthesis of Chiral Cyclic Ureas. ; _journal_issue 12 _journal_name_full 'ACS catalysis' _journal_page_first 11926 _journal_page_last 11931 _journal_paper_doi 10.1021/acscatal.8b03708 _journal_volume 8 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_moiety 'C24 H22 Br I N2 O4 S' _chemical_formula_sum 'C24 H22 Br I N2 O4 S' _chemical_formula_weight 641.30 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.4546(12) _cell_length_b 13.367(2) _cell_length_c 24.063(4) _cell_measurement_reflns_used 9880 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.86 _cell_volume 2397.8(7) _computing_cell_refinement 'APEX II v2014.11-0 (Bruker, 2014)' _computing_data_collection 'APEX II v2014.11-0 (Bruker, 2014)' _computing_data_reduction 'APEX II v2014.11-0 (Bruker, 2014)' _computing_molecular_graphics 'SHELXTL (Bruker, 2013)' _computing_publication_material 'SHELXTL (Bruker, 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELX (Bruker, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 83.33 _diffrn_detector_type 'Bruker APEXII' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details '0.50 degree frames measured for 10 seconds each' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_unetI/netI 0.0414 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 22668 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.529 _diffrn_reflns_theta_min 1.743 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 3.123 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, G. Sheldrick; 2014' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.777 _exptl_crystal_description plate _exptl_crystal_F_000 1264 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.041 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.078 _refine_ls_abs_structure_details ; Flack x determined using 2015 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.027(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 300 _refine_ls_number_reflns 5492 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0284 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0995P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.0694 _reflns_Friedel_coverage 0.754 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.992 _reflns_number_gt 5092 _reflns_number_total 5492 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b03708_si_003.cif _cod_data_source_block 16055 _cod_original_cell_volume 2397.7(7) _cod_database_code 4515776 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.444 _shelx_estimated_absorpt_t_max 0.859 _shelx_res_file ; 16055.res created by SHELXL-2014/7 TITL 16055 in P2(1)2(1)2(1) CELL 0.71073 7.4546 13.3666 24.0629 90.000 90.0000 90.0000 ZERR 4.00 0.0012 0.0021 0.0039 0.000 0.0000 0.0000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O S BR I UNIT 96 88 8 16 4 4 4 TEMP -123.160 ACTA SIZE 0.31 0.21 0.05 L.S. 20 FMAP 2 PLAN -5 0 0.00 HTAB HTAB C4 O1 EQIV $1 -x+1, y+1/2, -z+1/2 HTAB C9 O3_$1 HTAB C12 O3 EQIV $2 x+1/2, -y+3/2, -z HTAB C19 O4_$2 EQIV $3 x-1/2, -y+3/2, -z HTAB C24 I1_$3 HTAB C24 O2_$3 EQIV $4 -x+1, y-1/2, -z+1/2 HTAB C24 Br1_$4 BOND $H CONF WPDB -1 LIST 4 WGHT 0.034400 0.099500 FVAR 0.10199 I1 7 0.521314 1.087836 0.101507 11.00000 0.04204 0.04785 = 0.02042 0.00226 0.00358 0.00875 BR1 6 0.195506 0.968096 0.459187 11.00000 0.03813 0.04452 = 0.01908 0.00342 -0.00176 -0.01248 S1 5 0.798894 0.986679 0.240713 11.00000 0.01887 0.01762 = 0.02199 -0.00509 -0.00110 -0.00301 O1 4 0.739175 1.080865 0.261695 11.00000 0.02919 0.01780 = 0.03108 -0.00827 -0.00373 -0.00130 O2 4 0.948103 0.983304 0.203323 11.00000 0.02270 0.02840 = 0.02719 -0.00429 0.00028 -0.00739 O3 4 0.770063 0.805150 0.167332 11.00000 0.02266 0.02050 = 0.02457 -0.00877 0.00088 0.00208 O4 4 0.348389 0.562126 -0.017583 11.00000 0.03553 0.02155 = 0.02689 -0.00774 -0.00498 -0.00320 N1 3 0.620948 0.939140 0.207615 11.00000 0.01624 0.02168 = 0.02311 -0.00780 -0.00352 0.00115 N2 3 0.466714 0.833007 0.154979 11.00000 0.01961 0.02445 = 0.02256 -0.00925 0.00117 -0.00250 C1 1 0.434661 0.978951 0.211337 11.00000 0.01465 0.02627 = 0.02075 -0.00617 -0.00203 0.00341 C2 1 0.634644 0.852648 0.174691 11.00000 0.02090 0.01606 = 0.01745 -0.00321 0.00118 -0.00186 C3 1 0.329878 0.899905 0.176592 11.00000 0.02009 0.03522 = 0.02882 -0.01680 -0.00020 -0.00004 AFIX 23 H3A 2 0.243763 0.862987 0.200265 11.00000 -1.20000 H3B 2 0.263337 0.932371 0.145892 11.00000 -1.20000 AFIX 0 C4 1 0.418591 1.082970 0.185229 11.00000 0.02869 0.02892 = 0.01860 -0.00274 -0.00110 0.00639 AFIX 23 H4A 2 0.485265 1.131650 0.208356 11.00000 -1.20000 H4B 2 0.290879 1.103277 0.184957 11.00000 -1.20000 AFIX 0 C5 1 0.370289 0.978979 0.272124 11.00000 0.01558 0.02395 = 0.02393 -0.00721 -0.00259 -0.00116 C6 1 0.379301 0.890570 0.302230 11.00000 0.02201 0.02074 = 0.03111 -0.00159 0.00338 -0.00048 AFIX 43 H6 2 0.420916 0.831478 0.284483 11.00000 -1.20000 AFIX 0 C7 1 0.328511 0.886583 0.358061 11.00000 0.02307 0.02249 = 0.03893 0.00641 0.00155 -0.00256 AFIX 43 H7 2 0.337905 0.825920 0.378425 11.00000 -1.20000 AFIX 0 C8 1 0.264422 0.972329 0.383137 11.00000 0.02301 0.03114 = 0.01388 0.00157 -0.00294 -0.00651 C9 1 0.251159 1.061832 0.354236 11.00000 0.03026 0.02539 = 0.02068 -0.00382 0.00239 -0.00047 AFIX 43 H9 2 0.206682 1.120389 0.371865 11.00000 -1.20000 AFIX 0 C10 1 0.304612 1.063858 0.298723 11.00000 0.03275 0.01819 = 0.01804 0.00003 -0.00030 0.00280 AFIX 43 H10 2 0.295976 1.124748 0.278537 11.00000 -1.20000 AFIX 0 C11 1 0.838927 0.904797 0.296515 11.00000 0.01847 0.02060 = 0.02840 -0.00358 -0.00572 -0.00483 C12 1 0.931031 0.815906 0.289050 11.00000 0.02104 0.02401 = 0.03129 -0.00465 -0.00211 -0.00521 AFIX 43 H12 2 0.972830 0.797243 0.253224 11.00000 -1.20000 AFIX 0 C13 1 0.961582 0.754400 0.334491 11.00000 0.02425 0.02351 = 0.05006 0.00066 -0.00800 -0.00157 AFIX 43 H13 2 1.024229 0.693170 0.329477 11.00000 -1.20000 AFIX 0 C14 1 0.901648 0.781000 0.387677 11.00000 0.02877 0.03106 = 0.03806 0.00854 -0.00727 -0.01229 C15 1 0.806434 0.869053 0.393827 11.00000 0.02923 0.03782 = 0.02570 0.00136 -0.00151 -0.00897 AFIX 43 H15 2 0.762344 0.887109 0.429485 11.00000 -1.20000 AFIX 0 C16 1 0.773940 0.931773 0.348740 11.00000 0.02405 0.03155 = 0.02742 -0.00527 -0.00307 -0.00469 AFIX 43 H16 2 0.708390 0.992119 0.353496 11.00000 -1.20000 AFIX 0 C17 1 0.944472 0.716324 0.437865 11.00000 0.05258 0.03565 = 0.04654 0.01670 -0.01036 -0.00823 AFIX 137 H17A 2 0.919589 0.753974 0.471951 11.00000 -1.50000 H17B 2 1.071430 0.697359 0.437003 11.00000 -1.50000 H17C 2 0.870024 0.655916 0.437017 11.00000 -1.50000 AFIX 0 C18 1 0.435656 0.765035 0.109857 11.00000 0.02456 0.01629 = 0.01628 -0.00336 -0.00233 -0.00024 C19 1 0.550086 0.763557 0.065219 11.00000 0.02632 0.02380 = 0.03186 -0.00494 0.00270 -0.00936 AFIX 43 H19 2 0.647502 0.809319 0.063918 11.00000 -1.20000 AFIX 0 C20 1 0.525917 0.696474 0.022045 11.00000 0.02618 0.03003 = 0.02207 -0.00681 0.00334 -0.00433 AFIX 43 H20 2 0.608171 0.695158 -0.008101 11.00000 -1.20000 AFIX 0 C21 1 0.382153 0.631545 0.022888 11.00000 0.02665 0.01726 = 0.01769 -0.00170 -0.00666 -0.00106 C22 1 0.261175 0.635362 0.066447 11.00000 0.02994 0.01816 = 0.02678 -0.00158 -0.00339 -0.00879 AFIX 43 H22 2 0.159117 0.592801 0.066214 11.00000 -1.20000 AFIX 0 C23 1 0.287582 0.700848 0.110508 11.00000 0.02705 0.02771 = 0.01657 -0.00153 -0.00047 -0.00759 AFIX 43 H23 2 0.205839 0.702014 0.140790 11.00000 -1.20000 AFIX 0 C24 1 0.462826 0.564002 -0.065336 11.00000 0.03602 0.03360 = 0.02238 -0.01172 -0.00798 0.00501 AFIX 137 H24A 2 0.415712 0.518292 -0.093636 11.00000 -1.50000 H24B 2 0.583927 0.542935 -0.054649 11.00000 -1.50000 H24C 2 0.467190 0.632063 -0.080418 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM 16055 in P2(1)2(1)2(1) REM R1 = 0.0284 for 5092 Fo > 4sig(Fo) and 0.0322 for all 5492 data REM 300 parameters refined using 0 restraints END WGHT 0.0332 0.1822 REM Instructions for potential hydrogen bonds HTAB C4 O1 HTAB C9 O3_$1 HTAB C12 O3 HTAB C19 O4_$2 HTAB C24 I1_$3 HTAB C24 O2_$3 HTAB C24 Br1_$4 REM Highest difference peak 1.041, deepest hole -0.496, 1-sigma level 0.078 Q1 1 0.5751 1.0983 0.1286 11.00000 0.05 1.04 Q2 1 0.5551 1.0996 0.0712 11.00000 0.05 0.83 Q3 1 0.2102 0.9675 0.4224 11.00000 0.05 0.64 Q4 1 0.2750 0.9295 0.4568 11.00000 0.05 0.61 Q5 1 0.1879 0.9779 0.4915 11.00000 0.05 0.51 ; _shelx_res_checksum 66342 _shelx_hkl_file ; -1 0 0 0.43 0.08 -1 0 0 0.26 0.09 1 0 0 0.15 0.08 1 0 0 0.36 0.09 -2 0 0 -0.20 0.15 2 0 0 -0.02 0.15 -2 0 0 -0.16 0.14 -3 0 0 0.23 0.19 -3 0 0 0.16 0.20 3 0 0 0.20 0.20 4 0 0 237.90 14.67 -4 0 0 229.22 14.68 -4 0 0 243.67 14.66 -5 0 0 -0.04 0.32 -5 0 0 -0.02 0.30 5 0 0 -0.22 0.32 -6 0 0 23.77 1.85 -6 0 0 26.14 1.83 6 0 0 26.38 1.87 -7 0 0 1.09 0.97 7 0 0 0.36 0.53 -7 0 0 0.66 0.50 -7 0 0 0.54 0.48 -8 0 0 4.07 0.74 8 0 0 5.45 0.89 -8 0 0 5.31 0.89 -9 0 0 -0.18 0.50 -9 0 0 -0.27 0.72 9 0 0 -0.43 0.75 -1 1 0 0.43 0.11 -1 -1 0 0.37 0.11 1 -1 0 0.55 0.09 1 1 0 0.50 0.11 1 -1 0 0.57 0.12 -1 1 0 0.54 0.11 1 -1 0 0.46 0.09 -1 1 0 0.38 0.11 2 1 0 196.72 11.75 -2 1 0 192.11 11.73 -2 1 0 183.01 11.74 -2 1 0 182.74 11.74 -2 -1 0 196.24 11.75 -2 -1 0 198.54 11.76 2 -1 0 183.63 11.74 -3 1 0 50.68 3.09 -3 -1 0 46.34 3.11 -3 1 0 50.49 3.08 -3 -1 0 47.34 3.09 3 1 0 48.78 3.10 -3 1 0 47.37 3.09 3 -1 0 49.45 3.09 -4 1 0 22.57 1.47 -4 -1 0 17.37 1.44 -4 1 0 22.65 1.46 -4 1 0 23.80 1.45 4 1 0 17.28 1.45 4 -1 0 22.31 1.46 -5 1 0 36.72 2.56 -5 1 0 38.26 2.54 -5 -1 0 39.52 2.61 5 -1 0 38.32 2.57 -5 -1 0 40.51 2.57 -5 1 0 35.65 2.55 5 1 0 41.20 2.59 6 -1 0 24.61 1.79 -6 -1 0 23.64 1.75 -6 1 0 25.52 1.73 -6 1 0 22.06 1.69 -6 1 0 23.53 1.75 6 1 0 25.21 1.80 -6 -1 0 23.54 1.81 -7 1 0 1.51 0.54 -7 -1 0 3.44 0.65 7 1 0 4.13 0.71 7 -1 0 2.64 0.64 -7 1 0 2.98 0.63 -7 -1 0 3.56 0.70 -8 1 0 2.38 0.55 8 -1 0 3.04 0.76 -8 -1 0 2.31 0.77 8 1 0 1.89 0.73 -8 1 0 2.02 0.69 -9 1 0 13.50 1.23 -9 -1 0 13.99 1.45 9 1 0 17.46 1.69 -9 1 0 13.41 1.59 -9 -1 0 15.91 1.72 9 -1 0 16.28 1.68 1 2 0 465.34 27.91 -1 -2 0 445.91 27.89 -1 -2 0 450.68 27.98 -2 -2 0 167.86 11.55 2 -2 0 198.80 11.54 -2 2 0 196.41 11.52 2 2 0 179.70 11.55 -2 2 0 191.58 11.53 2 -2 0 200.09 11.54 -2 -2 0 174.14 11.56 -2 2 0 188.63 11.53 -3 2 0 52.10 3.20 -3 2 0 55.20 3.19 3 2 0 48.07 3.22 -3 2 0 50.02 3.20 -3 -2 0 49.11 3.24 -3 -2 0 47.04 3.21 3 -2 0 52.87 3.21 4 -2 0 20.43 1.38 -4 2 0 20.99 1.34 -4 2 0 18.85 1.36 -4 2 0 18.85 1.31 -4 2 0 18.72 1.34 -5 2 0 141.96 8.77 -5 -2 0 142.56 8.83 5 -2 0 140.47 8.82 5 2 0 145.82 8.85 -5 2 0 134.95 8.81 -5 2 0 138.46 8.81 -5 -2 0 138.66 8.87 -5 2 0 145.84 8.80 -6 2 0 28.13 2.04 -6 -2 0 30.56 2.23 6 -2 0 30.20 2.18 6 2 0 33.13 2.20 -6 2 0 30.87 2.10 -6 -2 0 32.68 2.18 -6 -2 0 31.22 2.28 -6 2 0 29.49 2.13 -7 -2 0 2.54 0.69 -7 -2 0 1.90 0.60 -7 2 0 1.25 0.52 7 -2 0 1.35 0.57 7 2 0 2.26 0.63 -7 2 0 1.38 0.39 -8 -2 0 2.50 0.80 -8 2 0 3.55 0.73 8 2 0 2.77 0.78 8 -2 0 4.19 0.82 -8 -2 0 2.41 0.73 -9 2 0 3.40 0.79 9 2 0 4.28 0.95 9 -2 0 3.65 0.94 -9 -2 0 2.70 0.94 -1 -3 0 173.09 10.85 -1 -3 0 175.35 10.84 1 3 0 178.72 10.83 2 3 0 25.84 1.59 2 -3 0 24.42 1.55 2 -3 0 23.75 1.56 2 -3 0 22.99 1.55 -2 -3 0 24.30 1.59 -2 -3 0 25.39 1.62 3 3 0 29.01 1.82 -3 3 0 29.08 1.75 -3 -3 0 27.88 1.82 -3 -3 0 28.28 1.86 -3 3 0 25.00 1.75 3 -3 0 27.31 1.79 -3 3 0 26.39 1.76 -4 -3 0 20.34 1.49 -4 3 0 19.66 1.43 -4 3 0 22.61 1.42 -4 -3 0 20.93 1.54 4 -3 0 22.24 1.47 4 3 0 20.70 1.49 -4 3 0 22.02 1.42 -5 3 0 0.95 0.28 -5 -3 0 0.29 0.42 -5 -3 0 0.68 0.39 -5 3 0 1.10 0.32 5 3 0 0.63 0.37 -5 -3 0 0.63 0.42 5 -3 0 0.31 0.34 -5 3 0 0.53 0.29 6 -3 0 9.57 1.01 -6 -3 0 11.18 1.10 -6 -3 0 9.92 1.13 -6 -3 0 9.67 1.03 -6 3 0 10.32 1.15 6 3 0 10.36 1.03 -6 3 0 10.08 0.94 -7 -3 0 1.18 0.60 7 -3 0 0.71 0.54 -7 -3 0 1.39 0.66 7 3 0 1.31 0.59 -7 3 0 1.21 0.47 -8 3 0 32.05 2.34 -8 -3 0 32.24 2.46 -8 -3 0 32.01 2.56 8 3 0 31.69 2.46 8 -3 0 33.63 2.46 -9 -3 0 0.29 0.87 -9 3 0 -0.08 0.58 9 3 0 -0.03 0.75 9 -3 0 -0.02 0.76 1 4 0 372.54 22.66 -1 -4 0 377.91 22.68 -1 -4 0 370.69 22.67 -1 -4 0 354.09 22.67 -2 -4 0 53.68 3.55 2 4 0 52.08 3.51 -2 -4 0 51.86 3.52 2 -4 0 58.14 3.47 2 -4 0 61.15 3.47 2 -4 0 58.60 3.53 3 -4 0 26.18 1.71 3 -4 0 24.41 1.70 -3 -4 0 27.77 1.80 3 -4 0 26.04 1.70 3 4 0 26.87 1.75 -3 -4 0 27.39 1.80 -3 -4 0 25.37 1.75 4 4 0 1.10 0.33 -4 -4 0 1.07 0.37 -4 -4 0 0.73 0.34 -4 -4 0 1.10 0.38 5 4 0 154.72 9.19 -5 -4 0 148.59 9.19 -5 -4 0 151.98 9.24 -5 4 0 134.07 9.09 -5 -4 0 156.84 9.28 -5 4 0 140.68 9.10 5 -4 0 139.75 9.14 -6 -4 0 6.81 0.90 -6 4 0 7.45 0.71 6 -4 0 6.10 0.84 -6 4 0 7.08 0.68 6 4 0 6.77 0.88 -6 -4 0 5.86 0.86 7 4 0 -0.04 0.54 -7 -4 0 -0.29 0.63 7 -4 0 0.08 0.52 -7 4 0 0.10 0.38 -7 -4 0 -0.23 0.57 8 -4 0 30.40 2.27 -8 -4 0 27.13 2.39 -8 -4 0 30.30 2.32 -8 4 0 28.75 2.08 8 4 0 27.22 2.25 -9 4 0 0.30 0.55 9 -4 0 0.09 0.75 -9 -4 0 -0.86 0.83 -9 -4 0 -0.71 0.83 9 4 0 -0.34 0.72 -1 -5 0 3.91 0.35 -1 -5 0 4.10 0.36 -2 -5 0 2.80 0.38 -2 -5 0 2.39 0.31 2 5 0 2.36 0.31 3 5 0 23.76 1.56 3 -5 0 22.49 1.51 3 -5 0 22.72 1.50 -3 -5 0 23.12 1.58 -3 -5 0 22.59 1.61 3 -5 0 22.42 1.50 -3 -5 0 24.25 1.62 -4 -5 0 52.67 3.34 -4 -5 0 52.28 3.35 4 -5 0 46.94 3.22 -4 -5 0 50.06 3.29 4 5 0 50.72 3.27 -5 -5 0 11.95 1.14 -5 -5 0 13.78 1.22 5 -5 0 14.57 1.08 5 5 0 12.81 1.12 -5 -5 0 12.37 1.21 6 5 0 0.69 0.48 -6 -5 0 1.15 0.61 -6 -5 0 0.57 0.53 -6 5 0 1.54 0.33 6 -5 0 1.37 0.47 -7 -5 0 18.82 1.69 7 -5 0 19.14 1.61 -7 -5 0 18.28 1.80 -7 5 0 19.67 1.39 7 5 0 19.14 1.62 8 5 0 5.36 0.92 -8 -5 0 4.70 1.05 8 -5 0 4.82 0.86 -8 5 0 5.40 0.75 -8 -5 0 6.26 1.02 -8 5 0 5.70 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7.10 1.14 -4 -4 -27 11.50 1.74 4 4 -27 10.27 1.54 -4 -4 -27 11.14 1.80 4 -4 -27 10.64 1.45 -4 -4 27 8.82 1.41 -4 4 -27 10.70 1.60 0 5 -27 14.26 1.68 0 -5 -27 15.18 1.81 0 -5 27 15.02 1.72 0 -5 -27 16.18 1.94 1 5 -27 5.90 1.09 -1 -5 -27 5.17 1.21 -1 -5 -27 4.85 1.23 1 -5 27 7.28 1.14 1 -5 -27 7.01 1.23 -1 -5 27 8.40 1.18 1 -5 -27 7.33 1.17 -1 5 -27 7.04 1.09 2 5 -27 12.55 1.72 -2 -5 -27 12.18 1.70 2 -5 27 12.32 1.68 -2 -5 -27 11.50 1.74 2 -5 -27 13.48 1.68 -2 5 -27 14.33 1.60 -2 -5 27 14.29 1.68 -3 -5 -27 5.83 1.46 3 -5 27 6.77 1.24 3 5 -27 4.48 1.15 -3 -5 -27 6.27 1.47 -3 -5 27 5.24 1.15 3 -5 -27 6.33 1.14 -3 5 -27 6.19 1.06 -4 -5 -27 2.12 1.36 4 -5 -27 4.70 1.13 -4 -5 27 3.91 1.13 0 6 -27 1.79 0.77 0 -6 -27 2.15 0.99 0 -6 27 2.20 0.88 1 6 -27 22.07 2.24 -1 -6 -27 23.53 2.48 -1 -6 -27 21.50 2.54 1 -6 27 24.30 2.26 -1 -6 27 30.58 2.33 -1 6 -27 28.20 2.21 1 -6 -27 28.96 2.38 2 6 -27 8.08 1.28 -2 -6 -27 9.46 1.60 -2 -6 -27 8.84 1.55 2 -6 27 10.32 1.35 2 -6 -27 8.13 1.29 -2 -6 27 7.51 1.26 -2 6 -27 9.62 1.32 3 6 -27 16.16 2.05 -3 -6 -27 19.88 2.55 -3 -6 -27 19.14 2.48 3 -6 27 19.22 2.15 -3 -6 27 18.69 2.04 3 -6 -27 20.23 2.03 -3 6 -27 18.40 1.75 0 -7 -27 23.25 2.31 0 -7 27 22.92 2.09 0 7 -27 19.57 1.94 -1 -7 -27 9.53 1.53 1 7 -27 8.53 1.26 1 -7 27 12.48 1.61 -1 7 -27 9.00 1.34 1 -7 -27 11.92 1.65 -1 -7 27 12.92 1.64 -2 -7 -27 3.75 1.36 2 -7 27 4.95 1.08 2 -7 -27 4.45 1.10 -2 7 -27 4.32 0.78 -2 -7 27 5.00 1.13 0 -8 -27 3.13 1.12 0 -8 27 3.73 0.99 1 -8 27 3.10 0.96 -1 -8 -27 3.03 1.24 -1 -8 27 3.75 0.99 1 -8 -27 3.61 1.09 -2 -8 -27 31.96 3.14 0 0 -28 45.94 3.49 0 0 -28 47.06 3.39 0 0 28 43.49 3.30 -1 0 28 1.84 0.72 1 0 28 1.30 0.76 -1 0 -28 0.52 0.82 -1 0 -28 2.29 0.93 1 0 -28 1.48 0.88 1 0 -28 1.54 0.80 2 0 -28 1.73 0.92 -2 0 -28 1.23 0.92 -2 0 -28 1.03 1.38 2 0 -28 2.51 0.88 -2 0 28 1.10 0.68 2 0 28 0.28 0.72 3 0 28 11.40 1.52 3 0 -28 14.62 1.84 -3 0 28 11.85 1.47 3 0 -28 14.83 1.69 -3 0 -28 12.10 1.63 -3 0 -28 10.07 1.44 -4 0 -28 6.89 1.36 4 0 -28 6.53 1.33 4 0 -28 6.35 1.22 -4 0 -28 6.10 1.02 4 0 28 8.07 1.41 0 1 -28 90.44 6.17 0 1 -28 90.57 6.26 0 -1 -28 94.72 6.22 0 -1 -28 92.87 6.31 0 1 28 93.43 6.15 0 -1 28 95.47 6.20 -1 -1 -28 7.63 1.27 -1 -1 -28 7.08 1.31 -1 1 28 10.48 1.30 1 1 -28 11.00 1.66 1 -1 28 8.47 1.22 1 1 -28 11.85 1.54 -1 1 -28 9.36 1.28 1 -1 -28 12.15 1.62 1 -1 -28 10.28 1.43 -1 -1 28 10.80 1.38 -1 1 -28 11.22 1.64 1 1 28 8.64 1.20 2 1 -28 1.23 0.89 2 -1 28 0.38 0.77 -2 -1 -28 0.67 0.93 -2 -1 -28 1.19 0.87 2 1 -28 1.46 0.81 -2 1 28 0.56 0.61 -2 1 -28 0.87 0.86 -2 1 -28 0.00 0.62 -2 -1 28 0.94 0.69 2 1 28 0.67 0.69 2 -1 -28 1.34 0.86 2 -1 -28 1.67 0.94 3 -1 28 7.96 1.31 3 1 -28 8.60 1.25 -3 -1 -28 8.51 1.39 3 1 -28 8.07 1.34 3 -1 -28 8.51 1.35 3 1 28 7.90 1.25 -3 1 -28 8.08 1.32 -3 1 -28 6.41 1.02 3 -1 -28 6.99 1.20 -3 -1 28 6.66 1.11 4 -1 28 17.44 2.22 -4 -1 -28 18.86 2.28 4 1 -28 17.46 2.14 4 1 -28 16.85 1.95 4 -1 -28 17.60 1.97 -4 1 -28 20.47 2.22 4 -1 -28 17.90 2.16 4 1 28 18.74 2.10 -4 -1 28 16.59 2.29 -4 1 -28 17.32 1.65 0 -2 -28 11.65 1.60 0 -2 28 11.71 1.54 0 2 -28 11.31 1.72 0 -2 -28 13.33 1.76 0 2 28 11.60 1.45 1 2 -28 14.25 1.72 -1 -2 -28 10.41 1.43 1 -2 28 12.50 1.56 -1 -2 -28 11.64 1.80 -1 2 28 13.36 1.55 1 -2 -28 9.75 1.36 1 -2 -28 10.91 1.72 -1 2 -28 11.05 1.64 1 2 28 10.75 1.42 -1 -2 28 10.77 1.47 -2 -2 -28 0.43 0.91 2 2 -28 1.03 0.85 2 -2 28 0.61 0.77 2 2 -28 0.54 0.84 -2 -2 -28 0.45 0.92 2 -2 -28 0.87 0.87 2 2 28 0.82 0.71 2 -2 -28 1.28 0.84 -2 -2 28 1.33 0.75 -2 2 -28 0.48 0.81 3 2 -28 7.54 1.36 3 -2 28 8.01 1.37 -3 -2 -28 8.58 1.49 -3 -2 -28 8.08 1.40 3 2 -28 8.32 1.34 -3 2 -28 12.55 1.69 -3 2 -28 8.67 1.16 3 -2 -28 9.92 1.45 -3 -2 28 10.21 1.35 3 2 28 9.16 1.32 3 -2 -28 9.36 1.33 4 2 -28 8.99 1.47 4 2 -28 9.47 1.72 4 -2 28 8.45 1.50 -4 -2 -28 8.53 1.57 4 2 28 8.32 1.37 -4 -2 28 8.24 1.29 4 -2 -28 9.23 1.40 -4 2 -28 8.40 1.13 -4 2 -28 9.67 1.42 4 -2 -28 8.24 1.44 0 -3 28 29.14 2.43 0 -3 -28 26.97 2.46 0 -3 -28 29.12 2.61 0 3 -28 29.43 2.52 -1 -3 -28 29.79 2.80 1 3 -28 33.58 2.71 1 -3 28 31.98 2.61 -1 -3 -28 28.69 2.65 -1 -3 28 32.21 2.59 1 -3 -28 32.87 2.78 1 3 28 30.21 2.60 1 -3 -28 32.85 2.65 -1 3 -28 33.74 2.71 2 3 -28 6.11 1.19 2 -3 28 6.51 1.17 -2 -3 -28 6.73 1.30 -2 -3 -28 6.59 1.25 2 3 28 6.03 1.04 2 -3 -28 6.34 1.17 2 -3 -28 7.27 1.26 -2 3 -28 8.10 1.19 -2 -3 28 6.16 1.11 -3 -3 -28 18.22 2.30 -3 -3 -28 17.87 2.17 3 -3 28 18.93 2.06 3 3 -28 17.36 2.02 -3 -3 28 17.03 1.88 3 -3 -28 17.94 2.01 3 -3 -28 19.20 2.11 3 3 28 14.93 1.85 -3 3 -28 17.26 1.98 0 4 -28 1.96 0.85 0 -4 28 1.29 0.81 0 -4 -28 0.75 0.91 0 -4 -28 0.44 0.91 1 -4 28 9.06 1.22 -1 -4 -28 6.50 1.30 1 4 -28 7.49 1.23 -1 -4 -28 7.17 1.23 1 -4 -28 5.81 1.21 -1 4 -28 6.60 1.14 -1 -4 28 6.92 1.14 1 -4 -28 5.75 1.16 2 4 -28 4.74 1.08 -2 -4 -28 3.90 1.20 2 -4 28 3.98 1.05 -2 -4 -28 5.39 1.29 -2 -4 28 4.53 1.02 2 -4 -28 3.75 1.08 -2 4 -28 4.73 1.03 2 -4 -28 5.50 1.12 -3 -4 -28 2.31 1.24 -3 -4 -28 3.33 1.31 3 4 -28 2.54 1.04 3 -4 28 2.41 1.04 -3 4 -28 3.89 0.99 -3 -4 28 3.94 1.03 3 -4 -28 3.57 1.05 0 -5 -28 1.06 0.96 0 -5 -28 1.07 0.95 0 5 -28 1.28 0.79 0 -5 28 1.24 0.86 -1 -5 -28 6.03 1.28 1 5 -28 5.99 1.14 -1 -5 -28 5.99 1.33 1 -5 28 6.69 1.17 -1 -5 28 8.43 1.23 -1 5 -28 9.87 1.43 1 -5 -28 7.83 1.35 1 -5 -28 7.62 1.24 2 -5 28 40.08 3.24 2 5 -28 38.00 3.23 -2 -5 -28 41.54 3.42 -2 -5 -28 39.00 3.50 -2 5 -28 45.01 3.17 2 -5 -28 41.83 3.21 -2 -5 28 43.26 3.23 3 -5 28 0.14 0.93 -3 -5 -28 1.27 1.20 -3 -5 -28 -0.07 1.13 3 5 -28 0.29 0.88 -3 5 -28 1.49 0.80 3 -5 -28 1.37 0.93 -3 -5 28 1.63 0.95 0 -6 28 5.13 1.08 0 -6 -28 4.95 1.16 0 6 -28 4.55 0.96 -1 -6 -28 0.55 1.08 1 6 -28 0.45 0.78 -1 -6 -28 1.16 1.07 1 -6 28 0.75 0.83 -1 6 -28 0.87 0.73 -1 -6 28 0.79 0.82 1 -6 -28 0.75 0.92 2 -6 28 12.94 1.75 -2 -6 -28 12.23 1.75 2 6 -28 9.69 1.45 -2 -6 -28 14.05 2.11 -2 6 -28 11.69 1.46 -2 -6 28 9.01 1.43 2 -6 -28 12.04 1.68 0 -7 -28 4.62 1.21 0 -7 28 6.16 1.11 0 7 -28 4.84 0.98 1 -7 28 0.78 0.84 1 7 -28 -0.07 0.74 -1 -7 -28 1.29 1.15 -1 7 -28 1.30 0.70 1 -7 -28 1.73 1.01 -1 -7 28 1.60 0.90 0 0 -29 1.25 0.93 0 0 29 0.87 0.70 0 0 -29 1.57 0.86 -1 0 29 7.32 1.08 1 0 -29 6.84 1.25 -1 0 -29 5.93 1.21 1 0 -29 6.94 1.13 -1 0 -29 6.05 1.14 1 0 29 6.60 1.09 2 0 -29 1.50 0.95 2 0 -29 2.16 0.90 -2 0 29 0.99 0.71 -2 0 -29 0.94 0.93 2 0 29 0.89 0.79 3 0 -29 1.49 0.92 3 0 29 0.68 0.87 -3 0 -29 1.30 1.03 3 0 -29 1.79 0.99 0 1 -29 6.53 1.20 0 -1 -29 6.54 1.24 0 -1 -29 5.92 1.12 0 1 29 5.88 1.04 0 -1 29 5.87 1.04 1 1 -29 26.24 2.26 1 -1 29 24.87 2.29 -1 -1 -29 25.57 2.44 -1 1 29 24.86 2.14 -1 -1 -29 25.69 2.31 1 1 -29 26.04 2.43 1 -1 -29 26.71 2.45 1 1 29 24.85 2.21 -1 -1 29 27.57 2.27 1 -1 -29 26.59 2.34 -1 1 -29 22.23 2.10 -1 1 -29 26.08 2.40 -2 -1 -29 15.38 1.82 2 1 -29 16.89 1.92 2 1 -29 15.45 1.72 2 -1 29 12.90 1.71 -2 -1 -29 14.04 2.00 2 1 29 14.62 1.74 -2 1 -29 12.69 1.89 2 -1 -29 13.36 1.89 -2 -1 29 14.80 1.67 -2 1 -29 11.54 1.47 2 -1 -29 14.60 1.82 -3 -1 -29 4.35 1.27 3 -1 29 6.62 1.22 3 1 -29 5.27 1.09 3 1 -29 5.76 1.22 -3 -1 29 5.16 1.01 3 1 29 4.85 1.10 3 -1 -29 5.14 1.12 3 -1 -29 4.62 1.18 -3 1 -29 5.55 1.21 -3 1 -29 3.96 0.86 0 2 -29 16.59 1.92 0 -2 -29 15.27 1.96 0 -2 29 14.97 1.79 0 -2 -29 16.73 1.89 0 2 29 14.25 1.65 1 2 -29 3.44 1.00 -1 -2 -29 2.29 1.00 -1 -2 -29 3.13 1.10 1 -2 29 2.42 0.90 1 -2 -29 3.24 1.05 1 -2 -29 3.27 0.97 -1 2 -29 2.86 0.95 1 2 29 2.67 0.82 -1 -2 29 2.72 0.86 -2 -2 -29 2.38 1.11 2 2 -29 2.18 0.95 2 -2 29 2.74 0.93 -2 -2 -29 2.00 1.01 2 -2 -29 3.39 1.07 2 -2 -29 3.36 0.99 2 2 29 2.39 0.85 -2 2 -29 2.48 0.97 -2 -2 29 2.80 0.88 3 2 -29 7.64 1.40 3 -2 29 9.18 1.42 -3 -2 -29 7.25 1.41 -3 -2 -29 9.24 1.57 3 -2 -29 13.16 1.65 3 2 29 9.82 1.36 -3 2 -29 10.49 1.45 3 -2 -29 12.70 1.83 -3 -2 29 10.69 1.49 0 3 -29 18.98 2.00 0 -3 29 18.69 1.91 0 -3 -29 18.28 2.12 0 -3 -29 17.78 1.98 1 -3 29 1.69 0.86 -1 -3 -29 2.20 1.06 -1 -3 -29 2.44 1.03 1 3 -29 2.17 0.92 1 -3 -29 1.17 0.94 -1 3 -29 2.41 0.96 -1 -3 29 1.01 0.77 1 -3 -29 1.83 0.95 -2 -3 -29 23.72 2.41 -2 -3 -29 23.54 2.46 2 3 -29 24.20 2.30 2 -3 29 21.75 2.19 2 -3 -29 22.12 2.20 2 -3 -29 24.14 2.40 -2 3 -29 21.62 2.24 -2 -3 29 23.05 2.16 -3 -3 -29 2.70 1.20 -3 -3 -29 3.40 1.28 3 -3 29 2.87 1.07 3 3 -29 3.50 1.04 -3 -3 29 2.44 0.93 -3 3 -29 2.96 0.99 3 -3 -29 2.57 1.06 0 -4 -29 12.66 1.85 0 -4 -29 15.63 1.94 0 -4 29 12.68 1.75 0 4 -29 14.94 1.78 -1 -4 -29 0.89 1.01 1 4 -29 1.07 0.87 1 -4 29 1.26 0.85 -1 -4 -29 0.67 0.99 -1 4 -29 1.77 0.87 1 -4 -29 1.33 0.94 -1 -4 29 1.45 0.84 1 -4 -29 1.10 0.97 2 4 -29 15.55 1.91 -2 -4 -29 14.77 2.19 -2 -4 -29 15.14 2.08 2 -4 29 12.54 1.89 2 -4 -29 17.97 2.03 -2 -4 29 16.86 1.86 -2 4 -29 17.54 1.91 2 -4 -29 17.64 1.95 0 -5 -29 0.15 0.95 0 -5 -29 0.19 0.94 0 -5 29 -0.17 0.80 0 5 -29 0.91 0.79 -1 -5 -29 24.35 2.37 -1 -5 -29 23.33 2.47 1 5 -29 22.32 2.19 1 -5 29 23.00 2.18 -1 -5 29 20.29 2.12 1 -5 -29 22.39 2.29 -1 5 -29 21.92 2.11 -2 -5 -29 2.94 1.23 2 -5 29 3.46 1.03 -2 -5 -29 2.44 1.25 2 5 -29 3.20 1.04 -2 5 -29 3.49 0.94 2 -5 -29 4.50 1.08 -2 -5 29 3.57 1.04 0 -6 -29 5.31 1.25 0 -6 29 5.75 1.11 0 6 -29 5.08 1.02 -1 -6 -29 3.04 1.18 1 -6 29 4.50 1.06 1 6 -29 2.15 0.93 -1 -6 -29 3.03 1.82 -1 -6 29 3.85 1.01 1 -6 -29 3.09 1.07 -1 6 -29 3.27 0.89 0 0 -30 38.12 3.14 0 0 -30 36.08 2.97 0 0 30 38.41 2.97 1 0 -30 21.03 2.29 -1 0 -30 21.88 2.29 1 0 -30 19.23 2.01 -1 0 30 20.82 1.98 1 0 30 18.86 2.00 2 0 -30 17.98 2.09 -2 0 -30 16.79 2.09 -2 0 30 15.73 1.71 2 0 -30 16.40 1.91 2 0 30 16.81 1.90 0 1 -30 1.15 0.93 0 -1 30 1.60 0.81 0 1 30 1.68 0.78 0 -1 -30 0.98 0.95 0 -1 -30 1.15 0.89 -1 -1 -30 2.01 1.00 1 -1 30 2.69 0.89 1 1 -30 2.25 1.00 -1 1 30 1.13 0.76 -1 -1 -30 0.96 0.93 -1 -1 30 1.62 0.78 -1 1 -30 1.75 0.98 1 -1 -30 2.40 1.02 1 -1 -30 1.94 0.91 1 1 30 1.09 0.78 -2 -1 -30 13.00 1.98 2 -1 30 13.34 1.75 2 1 -30 14.56 1.88 2 1 -30 12.40 1.86 2 -1 -30 14.38 1.97 2 1 30 13.57 1.74 -2 -1 30 12.24 1.56 2 -1 -30 13.33 1.70 -2 1 -30 13.15 1.90 -2 1 -30 9.80 1.42 0 -2 30 9.50 1.31 0 -2 -30 8.08 1.31 0 2 -30 11.40 1.71 0 -2 -30 8.05 1.42 1 -2 30 39.64 3.07 1 2 -30 39.88 3.15 -1 -2 -30 35.93 3.22 -1 -2 -30 40.61 3.09 -1 -2 30 39.55 3.02 1 2 30 37.64 3.03 1 -2 -30 35.52 3.14 1 -2 -30 37.02 3.05 -1 2 -30 38.23 3.12 -2 -2 -30 5.53 1.33 -2 -2 -30 5.70 1.24 2 -2 30 5.28 1.15 2 2 -30 5.25 1.21 2 -2 -30 8.51 1.26 2 2 30 6.24 1.12 2 -2 -30 8.80 1.43 -2 2 -30 7.13 1.27 -2 -2 30 8.39 1.23 0 3 -30 2.04 0.95 0 -3 -30 1.15 0.98 0 -3 -30 0.81 0.97 0 -3 30 1.53 0.87 1 -3 30 1.58 0.86 1 3 -30 1.37 0.88 -1 -3 -30 1.62 1.03 -1 -3 -30 0.55 1.03 -1 3 -30 1.06 0.90 1 -3 -30 1.26 0.94 -1 -3 30 1.70 0.85 1 -3 -30 1.39 0.99 -2 -3 -30 2.30 1.10 -2 -3 -30 1.94 1.17 2 -3 30 1.61 0.95 2 3 -30 3.32 1.05 -2 -3 30 3.30 0.97 -2 3 -30 3.35 1.05 2 -3 -30 4.28 1.18 2 -3 -30 3.65 1.05 0 4 -30 3.92 1.06 0 -4 30 5.02 1.08 0 -4 -30 5.59 1.21 0 -4 -30 5.11 1.25 1 4 -30 27.00 2.41 1 -4 30 27.19 2.43 -1 -4 -30 28.18 2.69 -1 -4 -30 26.25 2.49 -1 -4 30 24.20 2.31 -1 4 -30 26.06 2.38 1 -4 -30 22.57 2.36 1 -4 -30 23.77 2.50 0 0 31 0.51 0.75 1 0 31 4.32 1.01 1 0 -31 4.29 1.21 -1 0 -31 4.25 1.16 -1 0 31 3.27 0.92 1 0 -31 3.35 1.03 0 1 -31 5.76 1.26 0 -1 -31 4.41 1.11 0 -1 31 5.18 1.08 0 1 31 3.81 0.94 0 -1 -31 5.78 1.25 -1 -1 -31 5.25 1.36 1 -1 -31 5.56 1.13 0 -2 -31 2.97 1.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 32496 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 I1 I 0.52131(4) 1.08784(3) 0.10151(2) 0.03677(10) Uani 1 1 d . . Br1 Br 0.19551(6) 0.96810(4) 0.45919(2) 0.03391(13) Uani 1 1 d . . S1 S 0.79889(13) 0.98668(8) 0.24071(4) 0.0195(2) Uani 1 1 d . . O1 O 0.7392(4) 1.0809(2) 0.26170(12) 0.0260(6) Uani 1 1 d . . O2 O 0.9481(4) 0.9833(2) 0.20332(12) 0.0261(7) Uani 1 1 d . . O3 O 0.7701(4) 0.8051(2) 0.16733(12) 0.0226(6) Uani 1 1 d . . O4 O 0.3484(4) 0.5621(2) -0.01758(12) 0.0280(7) Uani 1 1 d . . N1 N 0.6209(4) 0.9391(3) 0.20762(14) 0.0203(8) Uani 1 1 d . . N2 N 0.4667(4) 0.8330(3) 0.15498(14) 0.0222(7) Uani 1 1 d . . C1 C 0.4347(5) 0.9790(4) 0.21134(16) 0.0206(9) Uani 1 1 d . . C2 C 0.6346(5) 0.8526(3) 0.17469(16) 0.0181(8) Uani 1 1 d . . C3 C 0.3299(5) 0.8999(4) 0.17659(18) 0.0280(10) Uani 1 1 d . . H3A H 0.2438 0.8630 0.2003 0.034 Uiso 1 1 calc R U H3B H 0.2633 0.9324 0.1459 0.034 Uiso 1 1 calc R U C4 C 0.4186(6) 1.0830(4) 0.18523(17) 0.0254(9) Uani 1 1 d . . H4A H 0.4853 1.1316 0.2084 0.030 Uiso 1 1 calc R U H4B H 0.2909 1.1033 0.1850 0.030 Uiso 1 1 calc R U C5 C 0.3703(5) 0.9790(3) 0.27212(17) 0.0212(9) Uani 1 1 d . . C6 C 0.3793(5) 0.8906(4) 0.30223(19) 0.0246(9) Uani 1 1 d . . H6 H 0.4209 0.8315 0.2845 0.030 Uiso 1 1 calc R U C7 C 0.3285(6) 0.8866(4) 0.3581(2) 0.0282(10) Uani 1 1 d . . H7 H 0.3379 0.8259 0.3784 0.034 Uiso 1 1 calc R U C8 C 0.2644(5) 0.9723(4) 0.38314(16) 0.0227(9) Uani 1 1 d . . C9 C 0.2512(6) 1.0618(4) 0.35424(18) 0.0254(10) Uani 1 1 d . . H9 H 0.2067 1.1204 0.3719 0.031 Uiso 1 1 calc R U C10 C 0.3046(6) 1.0639(3) 0.29872(17) 0.0230(9) Uani 1 1 d . . H10 H 0.2960 1.1247 0.2785 0.028 Uiso 1 1 calc R U C11 C 0.8389(5) 0.9048(3) 0.29651(17) 0.0225(9) Uani 1 1 d . . C12 C 0.9310(5) 0.8159(3) 0.28905(19) 0.0254(9) Uani 1 1 d . . H12 H 0.9728 0.7972 0.2532 0.031 Uiso 1 1 calc R U C13 C 0.9616(6) 0.7544(4) 0.3345(2) 0.0326(10) Uani 1 1 d . . H13 H 1.0242 0.6932 0.3295 0.039 Uiso 1 1 calc R U C14 C 0.9016(6) 0.7810(4) 0.3877(2) 0.0326(11) Uani 1 1 d . . C15 C 0.8064(6) 0.8691(4) 0.39383(19) 0.0309(10) Uani 1 1 d . . H15 H 0.7623 0.8871 0.4295 0.037 Uiso 1 1 calc R U C16 C 0.7739(6) 0.9318(4) 0.34874(18) 0.0277(10) Uani 1 1 d . . H16 H 0.7084 0.9921 0.3535 0.033 Uiso 1 1 calc R U C17 C 0.9445(8) 0.7163(4) 0.4379(2) 0.0449(14) Uani 1 1 d . . H17A H 0.9196 0.7540 0.4720 0.067 Uiso 1 1 calc R U H17B H 1.0714 0.6974 0.4370 0.067 Uiso 1 1 calc R U H17C H 0.8700 0.6559 0.4370 0.067 Uiso 1 1 calc R U C18 C 0.4357(5) 0.7650(3) 0.10986(16) 0.0190(8) Uani 1 1 d . . C19 C 0.5501(6) 0.7636(4) 0.06522(18) 0.0273(10) Uani 1 1 d . . H19 H 0.6475 0.8093 0.0639 0.033 Uiso 1 1 calc R U C20 C 0.5259(6) 0.6965(4) 0.02204(17) 0.0261(9) Uani 1 1 d . . H20 H 0.6082 0.6952 -0.0081 0.031 Uiso 1 1 calc R U C21 C 0.3822(6) 0.6315(3) 0.02289(16) 0.0205(8) Uani 1 1 d . . C22 C 0.2612(6) 0.6354(3) 0.06645(18) 0.0250(9) Uani 1 1 d . . H22 H 0.1591 0.5928 0.0662 0.030 Uiso 1 1 calc R U C23 C 0.2876(6) 0.7008(3) 0.11051(16) 0.0238(9) Uani 1 1 d . . H23 H 0.2058 0.7020 0.1408 0.029 Uiso 1 1 calc R U C24 C 0.4628(6) 0.5640(4) -0.06534(18) 0.0307(10) Uani 1 1 d . . H24A H 0.4157 0.5183 -0.0936 0.046 Uiso 1 1 calc R U H24B H 0.5839 0.5429 -0.0546 0.046 Uiso 1 1 calc R U H24C H 0.4672 0.6321 -0.0804 0.046 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 I1 0.04204(17) 0.0479(2) 0.02042(14) 0.00226(14) 0.00358(12) 0.00875(16) Br1 0.0381(2) 0.0445(3) 0.0191(2) 0.0034(2) -0.00176(18) -0.0125(2) S1 0.0189(4) 0.0176(5) 0.0220(5) -0.0051(4) -0.0011(4) -0.0030(4) O1 0.0292(14) 0.0178(15) 0.0311(16) -0.0083(14) -0.0037(12) -0.0013(14) O2 0.0227(14) 0.0284(18) 0.0272(15) -0.0043(14) 0.0003(12) -0.0074(14) O3 0.0227(14) 0.0205(15) 0.0246(15) -0.0088(13) 0.0009(11) 0.0021(12) O4 0.0355(16) 0.0215(17) 0.0269(15) -0.0077(13) -0.0050(13) -0.0032(14) N1 0.0162(15) 0.022(2) 0.0231(17) -0.0078(15) -0.0035(13) 0.0012(14) N2 0.0196(15) 0.0244(19) 0.0226(16) -0.0092(15) 0.0012(14) -0.0025(15) C1 0.0146(17) 0.026(2) 0.021(2) -0.0062(19) -0.0020(14) 0.0034(17) C2 0.0209(18) 0.016(2) 0.0175(19) -0.0032(17) 0.0012(15) -0.0019(17) C3 0.0201(19) 0.035(3) 0.029(2) -0.017(2) -0.0002(16) 0.0000(19) C4 0.029(2) 0.029(2) 0.0186(19) -0.003(2) -0.0011(16) 0.006(2) C5 0.0156(17) 0.024(2) 0.024(2) -0.0072(19) -0.0026(15) -0.0012(17) C6 0.0220(19) 0.021(2) 0.031(2) -0.0016(19) 0.0034(17) -0.0005(17) C7 0.023(2) 0.022(2) 0.039(2) 0.006(2) 0.0015(18) -0.0026(18) C8 0.0230(18) 0.031(2) 0.0139(18) 0.0016(18) -0.0029(14) -0.0065(18) C9 0.030(2) 0.025(2) 0.021(2) -0.0038(18) 0.0024(17) -0.0005(19) C10 0.033(2) 0.018(2) 0.0180(19) 0.0000(17) -0.0003(17) 0.0028(18) C11 0.0185(17) 0.021(2) 0.028(2) -0.004(2) -0.0057(15) -0.0048(18) C12 0.0210(19) 0.024(2) 0.031(2) -0.005(2) -0.0021(17) -0.0052(18) C13 0.024(2) 0.024(2) 0.050(3) 0.001(2) -0.008(2) -0.002(2) C14 0.029(2) 0.031(3) 0.038(3) 0.009(2) -0.0073(19) -0.012(2) C15 0.029(2) 0.038(3) 0.026(2) 0.001(2) -0.0015(19) -0.009(2) C16 0.024(2) 0.032(3) 0.027(2) -0.005(2) -0.0031(17) -0.0047(19) C17 0.053(3) 0.036(3) 0.047(3) 0.017(3) -0.010(3) -0.008(3) C18 0.0246(18) 0.0163(19) 0.0163(19) -0.0034(17) -0.0023(15) -0.0002(16) C19 0.026(2) 0.024(2) 0.032(2) -0.005(2) 0.0027(18) -0.0094(19) C20 0.026(2) 0.030(2) 0.0221(19) -0.0068(18) 0.0033(17) -0.004(2) C21 0.0266(19) 0.017(2) 0.0177(19) -0.0017(17) -0.0067(16) -0.0011(17) C22 0.030(2) 0.018(2) 0.027(2) -0.0016(18) -0.0034(17) -0.0088(19) C23 0.0271(19) 0.028(2) 0.017(2) -0.0015(18) -0.0005(16) -0.0076(19) C24 0.036(2) 0.034(3) 0.022(2) -0.0117(19) -0.0080(18) 0.005(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' S S 0.1246 0.1234 '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' I I -0.4742 1.8119 '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 O1 S1 O2 119.50(19) O1 S1 N1 104.84(18) O2 S1 N1 107.76(17) O1 S1 C11 109.4(2) O2 S1 C11 109.18(19) N1 S1 C11 105.18(19) C21 O4 C24 116.7(3) C2 N1 C1 113.3(3) C2 N1 S1 121.6(3) C1 N1 S1 125.1(3) C2 N2 C18 122.2(3) C2 N2 C3 113.7(3) C18 N2 C3 123.2(3) N1 C1 C4 111.9(3) N1 C1 C5 110.4(3) C4 C1 C5 111.4(3) N1 C1 C3 101.1(3) C4 C1 C3 110.9(3) C5 C1 C3 110.7(3) O3 C2 N2 128.0(4) O3 C2 N1 125.2(4) N2 C2 N1 106.7(3) N2 C3 C1 104.9(3) N2 C3 H3A 110.8 C1 C3 H3A 110.8 N2 C3 H3B 110.8 C1 C3 H3B 110.8 H3A C3 H3B 108.8 C1 C4 I1 112.5(3) C1 C4 H4A 109.1 I1 C4 H4A 109.1 C1 C4 H4B 109.1 I1 C4 H4B 109.1 H4A C4 H4B 107.8 C6 C5 C10 118.1(4) C6 C5 C1 118.7(4) C10 C5 C1 123.2(4) C5 C6 C7 121.4(4) C5 C6 H6 119.3 C7 C6 H6 119.3 C8 C7 C6 118.8(4) C8 C7 H7 120.6 C6 C7 H7 120.6 C7 C8 C9 121.4(4) C7 C8 Br1 119.3(3) C9 C8 Br1 119.3(3) C8 C9 C10 118.5(4) C8 C9 H9 120.8 C10 C9 H9 120.8 C5 C10 C9 121.7(4) C5 C10 H10 119.2 C9 C10 H10 119.2 C12 C11 C16 120.8(4) C12 C11 S1 121.3(3) C16 C11 S1 117.9(4) C11 C12 C13 119.2(4) C11 C12 H12 120.4 C13 C12 H12 120.4 C12 C13 C14 121.1(5) C12 C13 H13 119.4 C14 C13 H13 119.4 C15 C14 C13 118.5(4) C15 C14 C17 120.5(5) C13 C14 C17 121.0(5) C14 C15 C16 121.2(4) C14 C15 H15 119.4 C16 C15 H15 119.4 C15 C16 C11 119.1(4) C15 C16 H16 120.5 C11 C16 H16 120.5 C14 C17 H17A 109.5 C14 C17 H17B 109.5 H17A C17 H17B 109.5 C14 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C19 C18 C23 119.4(4) C19 C18 N2 120.1(4) C23 C18 N2 120.5(4) C18 C19 C20 121.1(4) C18 C19 H19 119.5 C20 C19 H19 119.5 C21 C20 C19 119.9(4) C21 C20 H20 120.1 C19 C20 H20 120.1 O4 C21 C20 124.0(4) O4 C21 C22 116.4(4) C20 C21 C22 119.6(4) C21 C22 C23 120.6(4) C21 C22 H22 119.7 C23 C22 H22 119.7 C22 C23 C18 119.3(4) C22 C23 H23 120.3 C18 C23 H23 120.3 O4 C24 H24A 109.5 O4 C24 H24B 109.5 H24A C24 H24B 109.5 O4 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance I1 C4 2.156(4) Br1 C8 1.902(4) S1 O1 1.428(3) S1 O2 1.431(3) S1 N1 1.673(3) S1 C11 1.758(5) O3 C2 1.206(5) O4 C21 1.368(5) O4 C24 1.431(5) N1 C2 1.405(5) N1 C1 1.490(5) N2 C2 1.364(5) N2 C18 1.435(5) N2 C3 1.453(5) C1 C4 1.530(7) C1 C5 1.539(5) C1 C3 1.557(6) C3 H3A 0.9900 C3 H3B 0.9900 C4 H4A 0.9900 C4 H4B 0.9900 C5 C6 1.388(6) C5 C10 1.392(6) C6 C7 1.397(6) C6 H6 0.9500 C7 C8 1.381(6) C7 H7 0.9500 C8 C9 1.387(6) C9 C10 1.394(6) C9 H9 0.9500 C10 H10 0.9500 C11 C12 1.384(6) C11 C16 1.394(6) C12 C13 1.387(7) C12 H12 0.9500 C13 C14 1.401(7) C13 H13 0.9500 C14 C15 1.382(7) C14 C17 1.519(7) C15 C16 1.392(7) C15 H15 0.9500 C16 H16 0.9500 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 C19 1.372(6) C18 C23 1.398(6) C19 C20 1.384(6) C19 H19 0.9500 C20 C21 1.379(6) C20 H20 0.9500 C21 C22 1.384(6) C22 C23 1.389(6) C22 H22 0.9500 C23 H23 0.9500 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 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 C4 H4A O1 0.99 2.39 3.016(5) 120.9 . C9 H9 O3 0.95 2.65 3.297(6) 125.9 3_655 C12 H12 O3 0.95 2.56 3.168(5) 121.8 . C19 H19 O4 0.95 2.54 3.419(5) 154.4 2_565 C24 H24A I1 0.98 3.27 3.963(5) 129.3 2_465 C24 H24A O2 0.98 2.65 3.382(5) 131.6 2_465 C24 H24B Br1 0.98 3.00 3.828(5) 143.4 3_645 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 O1 S1 N1 C2 171.0(3) O2 S1 N1 C2 42.7(4) C11 S1 N1 C2 -73.7(4) O1 S1 N1 C1 -11.8(4) O2 S1 N1 C1 -140.1(3) C11 S1 N1 C1 103.5(4) C2 N1 C1 C4 -116.0(4) S1 N1 C1 C4 66.6(4) C2 N1 C1 C5 119.3(4) S1 N1 C1 C5 -58.1(5) C2 N1 C1 C3 2.0(4) S1 N1 C1 C3 -175.3(3) C18 N2 C2 O3 -16.8(7) C3 N2 C2 O3 173.9(4) C18 N2 C2 N1 165.0(4) C3 N2 C2 N1 -4.3(5) C1 N1 C2 O3 -177.1(4) S1 N1 C2 O3 0.4(6) C1 N1 C2 N2 1.2(5) S1 N1 C2 N2 178.7(3) C2 N2 C3 C1 5.5(5) C18 N2 C3 C1 -163.7(4) N1 C1 C3 N2 -4.2(4) C4 C1 C3 N2 114.6(4) C5 C1 C3 N2 -121.2(4) N1 C1 C4 I1 52.7(4) C5 C1 C4 I1 176.8(2) C3 C1 C4 I1 -59.4(4) N1 C1 C5 C6 -53.8(5) C4 C1 C5 C6 -178.8(4) C3 C1 C5 C6 57.3(5) N1 C1 C5 C10 125.6(4) C4 C1 C5 C10 0.6(5) C3 C1 C5 C10 -123.3(4) C10 C5 C6 C7 -1.6(6) C1 C5 C6 C7 177.9(4) C5 C6 C7 C8 1.4(6) C6 C7 C8 C9 -0.6(6) C6 C7 C8 Br1 -179.8(3) C7 C8 C9 C10 -0.1(6) Br1 C8 C9 C10 179.1(3) C6 C5 C10 C9 0.9(6) C1 C5 C10 C9 -178.5(4) C8 C9 C10 C5 -0.1(6) O1 S1 C11 C12 -167.0(3) O2 S1 C11 C12 -34.5(4) N1 S1 C11 C12 80.9(4) O1 S1 C11 C16 13.4(4) O2 S1 C11 C16 145.9(3) N1 S1 C11 C16 -98.7(3) C16 C11 C12 C13 -1.3(6) S1 C11 C12 C13 179.1(3) C11 C12 C13 C14 -0.3(6) C12 C13 C14 C15 1.8(7) C12 C13 C14 C17 -176.5(4) C13 C14 C15 C16 -1.6(7) C17 C14 C15 C16 176.7(4) C14 C15 C16 C11 0.0(6) C12 C11 C16 C15 1.5(6) S1 C11 C16 C15 -178.9(3) C2 N2 C18 C19 -39.7(6) C3 N2 C18 C19 128.6(5) C2 N2 C18 C23 141.2(4) C3 N2 C18 C23 -50.5(6) C23 C18 C19 C20 -3.0(7) N2 C18 C19 C20 178.0(4) C18 C19 C20 C21 1.7(7) C24 O4 C21 C20 -5.2(6) C24 O4 C21 C22 174.2(4) C19 C20 C21 O4 -179.3(4) C19 C20 C21 C22 1.2(7) O4 C21 C22 C23 177.7(4) C20 C21 C22 C23 -2.9(7) C21 C22 C23 C18 1.6(7) C19 C18 C23 C22 1.3(6) N2 C18 C23 C22 -179.6(4)