#------------------------------------------------------------------------------ #$Date: 2019-11-23 18:51:17 +0200 (Sat, 23 Nov 2019) $ #$Revision: 234520 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/62/4036293.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_4036293 loop_ _publ_author_name 'Loh, Joanna K.' 'Asad, Naeem' 'Samarakoon, Thiwanka B.' 'Hanson, Paul R.' _publ_section_title ; Modular, One-Pot, Sequential Aziridine Ring Opening-S(N)Ar Strategy to 7-, 10-, and 11-Membered Benzo-Fused Sultams. ; _journal_issue 20 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 9926 _journal_page_last 9941 _journal_paper_doi 10.1021/acs.joc.5b01429 _journal_volume 80 _journal_year 2015 _chemical_absolute_configuration ad _chemical_formula_sum 'C15 H23 Br N2 O3 S' _chemical_formula_weight 391.32 _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 mixed _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.7849(7) _cell_length_b 11.4400(9) _cell_length_c 17.1570(14) _cell_measurement_reflns_used 9245 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.11 _cell_measurement_theta_min 4.65 _cell_volume 1724.3(2) _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 100(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker Platinum 135 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_unetI/netI 0.0245 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10088 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.100 _diffrn_reflns_theta_min 4.646 _diffrn_source 'Bruker MicroStar microfocus rotating anode' _exptl_absorpt_coefficient_mu 4.499 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.507 _exptl_crystal_description 'Rectangular parallelepiped' _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.486 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.052 _refine_ls_abs_structure_details ; Flack x determined using 1251 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.049(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 3067 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0246 _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^)+(0.0422P)^2^+0.6466P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.0684 _reflns_Friedel_coverage 0.706 _reflns_Friedel_fraction_full 0.974 _reflns_Friedel_fraction_max 0.951 _reflns_number_gt 3039 _reflns_number_total 3067 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo5b01429_si_002.cif _cod_data_source_block v26b_Cmpd_6a _cod_database_code 4036293 _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 0.533 _shelx_estimated_absorpt_t_max 0.774 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C15H23BrN2O3S CELL 1.54178 8.78490 11.44000 17.15700 90.0000 90.0000 90.0000 ZERR 4.00 0.00070 0.00090 0.00140 0.0000 0.0000 0.0000 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 S BR UNIT 60 92 8 12 4 4 TEMP -173.16C SIZE 0.06 0.10 0.16 L.S. 6 ACTA 132. WPDB -2 BOND $H CONF EQIV $1 -x+1, y-1/2, -z+1/2 EQIV $2 x-1/2, -y+1/2, -z EQIV $3 -x+1, y+1/2, -z+1/2 HTAB N1 O1 HTAB N1 N2 HTAB C2 O3 HTAB C2 N1_$1 HTAB C5 O2_$2 HTAB C11 O3 HTAB C15 O3_$3 HTAB FMAP -2 PLAN 20 WGHT 0.042200 0.646600 FVAR 0.17058 BR1 6 0.250394 -0.082526 -0.054893 11.00000 0.04337 0.02670 = 0.05354 -0.00909 -0.00049 -0.00096 S1 5 0.561957 0.264522 0.192453 11.00000 0.02685 0.03534 = 0.02381 0.00146 -0.00200 0.00576 O1 4 0.512565 0.312364 0.025288 11.00000 0.02698 0.02648 = 0.02605 0.00252 -0.00018 -0.00126 O2 4 0.534542 0.211112 0.266666 11.00000 0.04204 0.04428 = 0.02460 0.00644 0.00013 0.01148 O3 4 0.715443 0.293846 0.171782 11.00000 0.02564 0.04953 = 0.03169 -0.00111 -0.00344 0.00436 N1 3 0.464190 0.384925 0.187899 11.00000 0.02454 0.02977 = 0.02447 0.00203 0.00048 0.00106 H1N 2 0.497420 0.420002 0.156798 11.00000 0.02049 N2 3 0.328593 0.511205 0.070985 11.00000 0.02967 0.02218 = 0.02734 0.00041 -0.00034 -0.00013 C1 1 0.485082 0.167493 0.121900 11.00000 0.02523 0.02846 = 0.02777 0.00103 0.00480 0.00760 C2 1 0.446054 0.054500 0.144757 11.00000 0.03456 0.03089 = 0.03191 0.00441 0.00683 0.00800 H2 2 0.464444 0.037689 0.198287 11.00000 0.03373 C3 1 0.380092 -0.021877 0.092102 11.00000 0.03518 0.02486 = 0.04378 0.00431 0.01152 0.00396 H3 2 0.360423 -0.099962 0.107600 11.00000 0.02475 C4 1 0.349263 0.018110 0.017699 11.00000 0.02797 0.02442 = 0.04137 -0.00531 0.00275 0.00323 C5 1 0.385957 0.130242 -0.007275 11.00000 0.02597 0.02757 = 0.03003 -0.00096 0.00148 0.00567 H5 2 0.368869 0.152070 -0.054566 11.00000 0.02242 C6 1 0.458687 0.204669 0.045059 11.00000 0.02293 0.02070 = 0.02957 -0.00040 0.00361 0.00408 C7 1 0.427810 0.380858 -0.031038 11.00000 0.03538 0.02580 = 0.02104 0.00317 -0.00180 -0.00233 H7A 2 0.502575 0.445891 -0.047723 11.00000 0.03830 H7B 2 0.404825 0.330380 -0.076306 11.00000 0.02765 C8 1 0.287608 0.431504 0.007488 11.00000 0.03228 0.02634 = 0.02558 0.00240 -0.00464 -0.00145 H8A 2 0.237027 0.471703 -0.033735 11.00000 0.04299 H8B 2 0.229327 0.367834 0.025548 11.00000 0.02536 C9 1 0.244399 0.491956 0.143057 11.00000 0.02771 0.02598 = 0.02683 -0.00290 0.00198 0.00191 H9A 2 0.267177 0.551929 0.175024 11.00000 0.02618 H9B 2 0.137614 0.486609 0.132823 11.00000 0.02266 C10 1 0.295115 0.378169 0.183004 11.00000 0.02403 0.02671 = 0.02392 -0.00121 -0.00099 0.00104 H10 2 0.261703 0.310399 0.151577 11.00000 0.01762 C11 1 0.218307 0.362554 0.262524 11.00000 0.02555 0.03042 = 0.02481 -0.00274 -0.00016 0.00046 H11A 2 0.280326 0.314082 0.293884 11.00000 0.02398 H11B 2 0.214388 0.436591 0.289044 11.00000 0.02892 C12 1 0.058578 0.309135 0.255101 11.00000 0.02625 0.03800 = 0.02271 0.00102 0.00362 -0.00017 H12 2 -0.002725 0.349771 0.209488 11.00000 0.02297 C13 1 0.065857 0.179389 0.235277 11.00000 0.03708 0.03497 = 0.03149 -0.00239 0.00324 -0.00742 H13A 2 -0.028915 0.146124 0.230207 11.00000 0.03650 H13B 2 0.118612 0.134243 0.277896 11.00000 0.04539 H13C 2 0.114485 0.163948 0.187303 11.00000 0.05433 C14 1 -0.032331 0.325931 0.329662 11.00000 0.03210 0.04514 = 0.03120 -0.00441 0.00646 -0.00154 H14A 2 -0.048077 0.397585 0.338378 11.00000 0.03958 H14B 2 -0.127496 0.295475 0.324218 11.00000 0.04184 H14C 2 0.019915 0.295324 0.373383 11.00000 0.04600 C15 1 0.325350 0.632939 0.046586 11.00000 0.04589 0.02654 = 0.03512 0.00061 0.00267 0.00122 AFIX 137 H15A 2 0.220029 0.656371 0.036081 11.00000 0.03585 H15B 2 0.386324 0.642342 -0.000833 11.00000 0.03056 H15C 2 0.367512 0.682125 0.088071 11.00000 0.06198 AFIX 0 HKLF 4 REM C15H23BrN2O3S REM R1 = 0.0246 for 3039 Fo > 4sig(Fo) and 0.0247 for all 3067 data REM 283 parameters refined using 0 restraints END WGHT 0.0421 0.6517 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB N1 N2 HTAB C2 O2 HTAB C2 N1_$1 HTAB C5 O3_$2 HTAB C11 O2 HTAB C15 O2_$3 REM Highest difference peak 0.486, deepest hole -0.371, 1-sigma level 0.052 Q1 1 0.3550 -0.0954 -0.0533 11.00000 0.05 0.49 Q2 1 0.2438 -0.0389 -0.1020 11.00000 0.05 0.39 Q3 1 0.2674 -0.0913 -0.0773 11.00000 0.05 -0.37 Q4 1 0.2077 -0.0643 -0.0564 11.00000 0.05 -0.36 Q5 1 0.2669 -0.0983 -0.0255 11.00000 0.05 -0.35 Q6 1 0.1310 -0.1207 -0.0588 11.00000 0.05 0.32 Q7 1 0.6633 0.2543 0.1847 11.00000 0.05 0.31 Q8 1 0.1353 0.3352 0.2604 11.00000 0.05 0.23 Q9 1 0.4487 0.2763 0.0384 11.00000 0.05 0.22 Q10 1 0.2431 -0.1739 -0.0567 11.00000 0.05 0.22 Q11 1 0.3631 0.2698 0.1953 11.00000 0.05 -0.21 Q12 1 0.3459 -0.0016 0.0592 11.00000 0.05 0.20 Q13 1 0.5271 0.2118 0.1581 11.00000 0.05 0.19 Q14 1 0.4982 0.1045 0.1279 11.00000 0.05 0.19 Q15 1 0.4551 0.1595 0.0208 11.00000 0.05 0.18 Q16 1 0.4932 0.0185 0.1221 11.00000 0.05 0.18 Q17 1 0.2648 0.4354 0.1603 11.00000 0.05 0.17 Q18 1 0.4680 0.1797 0.0799 11.00000 0.05 0.17 Q19 1 0.3820 0.3812 0.1944 11.00000 0.05 0.17 Q20 1 0.5256 0.3285 0.1823 11.00000 0.05 0.17 ; _shelx_res_checksum 89377 _shelx_hkl_file ; -1 0 0 0.28 0.03 -2 0 0 10.51 0.49 2 0 0 10.19 0.53 4 0 0 694.03 26.56 4 0 0 749.01 30.45 5 0 0 -0.05 0.05 5 0 0 -0.03 0.06 6 0 0 129.80 5.68 6 0 0 131.70 4.97 7 0 0 -0.05 0.07 7 0 0 -0.01 0.11 8 0 0 3.34 0.26 8 0 0 3.37 0.24 8 0 0 3.25 0.25 8 0 0 2.98 0.18 9 0 0 0.11 0.08 9 0 0 0.05 0.04 9 0 0 0.07 0.09 10 0 0 42.67 1.54 10 0 0 40.30 1.53 0 -1 0 0.01 0.01 -1 -1 0 58.31 2.42 2 -1 0 62.13 2.65 -2 1 0 61.29 2.48 -2 -1 0 61.59 2.51 2 1 0 61.74 2.64 -3 -1 0 1.74 0.13 3 -1 0 1.80 0.15 3 1 0 2.14 0.15 4 1 0 8.71 0.42 4 1 0 8.47 0.35 -4 -1 0 8.88 0.43 4 -1 0 8.87 0.47 4 -1 0 8.01 0.40 4 1 0 8.53 0.46 5 -1 0 54.88 2.13 5 1 0 53.91 2.13 5 1 0 54.82 2.42 5 -1 0 54.01 2.44 6 -1 0 24.18 1.23 6 1 0 25.08 1.09 6 -1 0 25.66 1.09 6 1 0 24.76 1.21 7 1 0 60.02 1.96 7 -1 0 60.88 1.96 8 -1 0 1.30 0.17 8 -1 0 1.14 0.17 8 -1 0 1.33 0.16 8 -1 0 1.27 0.11 8 1 0 1.13 0.18 8 1 0 1.21 0.17 9 1 0 34.10 1.35 9 -1 0 36.18 1.37 9 -1 0 35.17 1.34 9 1 0 36.29 1.38 9 -1 0 34.98 1.37 9 1 0 35.26 1.36 10 -1 0 4.25 0.26 10 1 0 4.55 0.27 10 1 0 4.71 0.22 0 -2 0 11.99 0.51 -1 -2 0 5.68 0.27 -2 -2 0 989.22 39.88 2 -2 0 1000.00 41.95 3 -2 0 0.01 0.04 3 2 0 0.01 0.04 3 2 0 0.08 0.04 -3 -2 0 -0.01 0.03 -4 -2 0 2.08 0.17 4 2 0 2.03 0.16 4 2 0 2.02 0.17 4 2 0 2.00 0.12 4 -2 0 1.91 0.15 4 -2 0 2.08 0.18 5 2 0 0.72 0.13 5 -2 0 0.72 0.11 5 -2 0 0.74 0.14 5 2 0 0.86 0.13 6 -2 0 4.54 0.36 7 -2 0 9.85 0.45 8 -2 0 57.39 1.86 8 2 0 54.91 2.07 8 -2 0 57.36 2.17 8 2 0 55.36 2.09 8 -2 0 55.71 2.09 8 -2 0 55.53 2.06 8 -2 0 55.41 2.08 9 2 0 0.32 0.11 9 -2 0 0.29 0.06 9 -2 0 0.33 0.10 9 -2 0 0.35 0.11 9 2 0 0.27 0.06 9 2 0 0.29 0.10 10 2 0 0.85 0.09 10 2 0 0.80 0.12 0 -3 0 0.00 0.03 1 -3 0 0.90 0.07 -1 -3 0 1.04 0.10 2 3 0 158.99 5.93 2 3 0 159.24 5.93 2 -3 0 159.06 6.80 -2 -3 0 162.85 6.47 3 -3 0 0.46 0.05 -3 -3 0 0.50 0.10 4 3 0 111.79 4.31 4 -3 0 117.17 5.00 -4 -3 0 116.87 4.75 4 -3 0 117.44 4.37 5 -3 0 6.52 0.42 5 -3 0 6.54 0.37 -5 -3 0 6.22 0.39 5 3 0 6.17 0.30 6 -3 0 62.01 2.81 7 -3 0 0.06 0.08 8 -3 0 0.07 0.05 8 -3 0 0.05 0.08 8 -3 0 0.07 0.11 8 -3 0 0.10 0.08 8 3 0 0.05 0.08 8 3 0 0.08 0.06 9 3 0 0.81 0.13 9 -3 0 0.76 0.09 9 -3 0 0.68 0.12 9 3 0 0.78 0.11 10 3 0 0.15 0.05 10 3 0 0.14 0.08 0 -4 0 42.61 1.76 1 -4 0 10.93 0.48 -1 -4 0 11.43 0.52 2 4 0 74.29 2.77 2 4 0 74.60 2.77 2 -4 0 70.73 2.75 -2 -4 0 73.38 3.03 3 -4 0 11.31 0.57 3 -4 0 10.98 0.52 -3 -4 0 11.53 0.57 3 -4 0 11.42 0.47 3 4 0 11.23 0.50 4 4 0 49.54 1.88 4 -4 0 48.87 1.93 4 -4 0 48.13 2.18 -4 -4 0 47.98 2.09 5 -4 0 1.13 0.17 5 4 0 1.00 0.11 6 -4 0 4.84 0.31 7 4 0 3.13 0.23 7 4 0 2.91 0.25 7 -4 0 2.71 0.23 7 -4 0 3.13 0.25 7 -4 0 2.80 0.19 8 -4 0 21.13 0.93 8 -4 0 21.48 0.82 8 -4 0 20.58 0.85 8 4 0 21.63 0.91 8 4 0 21.53 0.91 9 4 0 0.26 0.09 9 4 0 0.20 0.07 9 -4 0 0.20 0.09 10 4 0 3.06 0.18 10 4 0 2.93 0.20 0 -5 0 -0.02 0.03 0 -5 0 -0.02 0.05 -1 -5 0 50.61 2.06 -1 -5 0 47.94 1.92 1 -5 0 48.95 1.90 2 -5 0 21.10 0.91 2 5 0 21.21 0.86 2 5 0 21.56 0.89 2 5 0 21.53 0.89 -2 -5 0 21.43 0.98 2 -5 0 21.75 0.87 3 -5 0 216.35 8.22 3 -5 0 223.51 8.15 3 5 0 225.13 8.18 -3 -5 0 221.10 8.94 3 5 0 214.84 7.98 -4 -5 0 40.51 1.81 4 5 0 41.26 1.62 5 5 0 17.28 0.75 6 5 0 2.68 0.20 6 -5 0 2.80 0.23 6 -5 0 2.81 0.23 7 5 0 71.82 2.68 7 -5 0 67.99 2.60 7 -5 0 68.40 2.26 7 5 0 71.46 2.56 7 -5 0 66.70 2.58 8 5 0 0.56 0.14 8 -5 0 0.77 0.14 8 5 0 0.88 0.14 8 -5 0 0.59 0.09 9 5 0 16.11 0.70 9 -5 0 15.68 0.62 9 5 0 16.68 0.70 0 -6 0 27.08 1.12 1 -6 0 11.73 0.54 1 6 0 11.36 0.52 -1 -6 0 11.44 0.57 -1 -6 0 11.08 0.55 2 6 0 138.72 5.23 -2 -6 0 135.41 5.69 2 -6 0 140.97 5.21 2 6 0 139.52 5.23 2 -6 0 135.85 5.25 2 6 0 142.54 5.10 3 6 0 23.69 0.99 3 6 0 23.31 0.94 3 -6 0 23.55 0.95 -3 -6 0 23.12 1.10 3 -6 0 22.85 1.02 4 6 0 101.72 3.88 5 -6 0 0.39 0.12 5 6 0 0.45 0.11 6 -6 0 115.82 3.71 6 6 0 114.84 4.44 6 -6 0 115.92 4.36 6 -6 0 123.68 3.80 7 -6 0 0.53 0.09 7 -6 0 0.49 0.14 7 -6 0 0.53 0.13 7 6 0 0.72 0.15 8 6 0 1.86 0.20 8 -6 0 1.94 0.14 8 6 0 1.63 0.18 8 -6 0 2.13 0.19 9 6 0 7.09 0.37 9 6 0 7.24 0.36 0 -7 0 0.08 0.07 1 -7 0 269.10 10.13 -1 -7 0 268.81 10.16 1 -7 0 280.67 10.16 1 7 0 270.76 9.92 2 7 0 0.65 0.13 2 -7 0 0.82 0.12 2 7 0 0.72 0.11 -2 -7 0 0.69 0.14 3 7 0 119.65 4.37 3 -7 0 116.99 4.45 3 7 0 117.52 4.51 4 -7 0 2.20 0.21 4 7 0 2.31 0.23 5 -7 0 123.11 3.94 5 7 0 124.04 4.77 5 -7 0 128.53 4.04 6 -7 0 1.57 0.15 6 -7 0 1.45 0.18 6 7 0 1.61 0.21 6 -7 0 1.50 0.22 7 7 0 10.82 0.55 7 -7 0 11.01 0.49 7 -7 0 10.51 0.51 7 -7 0 10.76 0.49 8 -7 0 1.71 0.13 8 -7 0 1.73 0.16 8 7 0 1.72 0.18 0 -8 0 6.93 0.42 1 -8 0 14.62 0.71 -1 -8 0 13.87 0.73 1 -8 0 15.65 0.73 1 8 0 14.63 0.68 2 -8 0 1.41 0.18 2 -8 0 1.39 0.18 2 -8 0 1.75 0.21 2 8 0 1.49 0.16 3 -8 0 3.73 0.27 3 -8 0 3.60 0.26 3 8 0 3.73 0.26 3 -8 0 4.18 0.28 3 8 0 3.90 0.31 4 -8 0 88.11 2.74 4 -8 0 84.58 2.81 4 8 0 81.92 3.32 5 -8 0 3.87 0.27 5 -8 0 3.52 0.29 5 -8 0 3.46 0.25 6 -8 0 3.61 0.29 6 -8 0 3.92 0.27 6 -8 0 3.90 0.25 7 -8 0 4.25 0.24 7 -8 0 3.82 0.28 7 8 0 3.99 0.28 7 -8 0 4.43 0.26 8 8 0 12.55 0.57 8 -8 0 13.75 0.54 0 -9 0 0.13 0.10 0 -9 0 -0.03 0.08 0 9 0 -0.02 0.09 -1 -9 0 1.25 0.22 1 -9 0 1.60 0.21 1 -9 0 1.27 0.18 1 -9 0 1.45 0.17 -1 -9 0 1.55 0.18 1 -9 0 1.40 0.20 1 9 0 1.29 0.18 -2 -9 0 0.83 0.15 2 -9 0 1.13 0.17 2 -9 0 0.85 0.16 2 9 0 0.95 0.20 2 -9 0 0.90 0.15 2 9 0 1.10 0.17 3 9 0 0.25 0.10 3 -9 0 0.28 0.12 3 9 0 0.11 0.11 3 -9 0 0.30 0.11 3 9 0 0.27 0.13 -3 -9 0 0.29 0.12 3 -9 0 0.16 0.09 4 -9 0 0.51 0.13 4 -9 0 0.43 0.10 4 -9 0 0.37 0.12 5 -9 0 3.76 0.30 5 -9 0 4.33 0.28 5 -9 0 4.14 0.27 6 -9 0 1.32 0.14 6 -9 0 1.30 0.16 6 -9 0 1.15 0.17 7 -9 0 2.91 0.18 7 -9 0 3.00 0.22 7 -9 0 3.08 0.19 0 -10 0 39.04 1.43 0 10 0 40.05 1.60 0 -10 0 39.37 1.33 0 -10 0 37.26 1.63 0 10 0 38.18 1.48 1 10 0 3.95 0.30 1 10 0 3.80 0.32 -1 -10 0 3.98 0.28 1 -10 0 3.81 0.28 -1 -10 0 3.81 0.26 1 -10 0 3.83 0.26 -2 -10 0 14.95 0.62 2 10 0 14.31 0.71 2 -10 0 14.91 0.61 2 10 0 14.60 0.70 2 -10 0 14.75 0.63 -2 -10 0 14.27 0.64 3 10 0 10.32 0.57 3 -10 0 10.29 0.50 3 -10 0 10.67 0.47 -3 -10 0 10.79 0.49 3 10 0 10.01 0.51 -3 -10 0 10.28 0.51 4 10 0 19.79 0.87 4 -10 0 20.58 0.82 -4 -10 0 20.16 0.83 -4 -10 0 20.36 0.79 4 -10 0 20.51 0.77 5 -10 0 2.35 0.19 5 -10 0 2.38 0.23 5 -10 0 2.56 0.20 -5 -10 0 2.69 0.21 -5 -10 0 2.71 0.22 6 -10 0 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1.60 0.14 9 2 3 1.88 0.19 9 2 3 1.58 0.18 9 2 3 1.62 0.13 9 -2 -3 1.52 0.18 10 2 -3 9.58 0.42 10 2 -3 9.27 0.44 10 -2 -3 10.05 0.40 10 2 3 9.93 0.38 10 2 3 9.20 0.44 10 -2 -3 8.72 0.43 10 2 3 9.81 0.45 0 -3 -3 16.39 0.72 0 -3 3 16.31 0.70 1 -3 3 102.07 4.93 1 -3 3 107.72 4.67 -1 -3 -3 114.40 4.71 1 -3 -3 124.12 4.68 -1 -3 3 123.49 4.70 1 -3 -3 123.42 4.94 -2 -3 -3 13.51 0.64 2 -3 3 12.80 0.65 2 -3 3 13.03 0.54 2 3 -3 13.03 0.57 2 -3 -3 14.47 0.66 -2 -3 3 14.56 0.63 2 3 3 13.49 0.53 2 -3 -3 13.95 0.58 2 3 3 14.03 0.58 3 -3 3 265.13 11.31 -3 -3 -3 269.23 10.77 3 3 -3 267.80 9.85 3 -3 3 261.91 9.89 -3 -3 3 268.85 10.75 3 3 3 268.94 9.84 3 -3 -3 261.28 9.84 3 -3 -3 269.01 11.32 4 3 -3 94.14 3.43 4 -3 3 94.31 3.48 -4 -3 -3 92.10 3.79 4 -3 3 94.69 3.97 4 -3 -3 88.30 3.97 -4 -3 3 89.84 3.76 4 3 3 85.29 3.40 4 -3 -3 89.35 3.41 5 -3 3 38.74 1.59 -5 -3 -3 37.11 1.72 5 -3 3 39.22 1.81 5 3 -3 38.96 1.52 5 -3 -3 40.00 1.83 -5 -3 3 39.44 1.71 6 -3 3 6.10 0.32 6 -3 3 5.92 0.40 6 -3 3 6.13 0.44 6 3 -3 5.88 0.31 6 -3 -3 7.00 0.47 7 -3 3 81.75 2.98 7 -3 3 80.42 3.31 7 -3 3 83.10 2.67 7 -3 3 85.01 3.51 7 3 3 88.10 3.02 8 -3 3 30.63 1.15 8 3 -3 30.68 1.19 8 -3 3 29.64 1.14 8 3 -3 30.54 1.18 8 -3 3 30.49 1.05 8 -3 3 30.76 1.24 8 -3 3 29.56 1.39 8 3 3 28.17 1.19 8 3 3 27.40 1.16 8 3 3 29.04 1.17 8 -3 -3 28.10 1.18 8 -3 -3 26.83 1.16 9 3 -3 15.24 0.68 9 -3 3 15.47 0.72 9 3 -3 14.47 0.66 9 -3 3 15.09 0.65 9 -3 3 15.62 0.61 9 3 3 15.11 0.69 9 -3 -3 16.02 0.65 9 3 3 15.85 0.65 9 3 3 15.13 0.67 9 -3 -3 15.85 0.68 10 3 -3 1.94 0.16 10 3 -3 1.87 0.14 10 -3 -3 1.73 0.15 10 3 3 1.64 0.15 10 3 3 1.87 0.11 0 -4 3 144.86 5.38 0 -4 3 148.37 5.84 0 -4 -3 138.25 5.40 0 -4 -3 146.40 5.85 1 -4 3 39.23 1.55 -1 -4 -3 40.79 1.67 1 -4 3 41.34 1.51 -1 -4 3 39.78 1.66 1 4 3 38.11 1.53 -1 -4 3 37.78 1.53 1 -4 -3 38.48 1.54 2 -4 3 110.73 4.20 2 4 -3 112.69 4.17 2 -4 3 111.37 4.13 -2 -4 -3 115.03 4.57 2 4 3 111.55 4.18 -2 -4 3 111.12 4.54 2 -4 -3 108.90 4.17 2 4 3 108.36 3.77 3 4 -3 41.50 1.57 3 -4 3 41.46 1.61 3 4 -3 40.73 1.52 -3 -4 -3 42.10 1.75 3 -4 3 40.99 1.80 3 -4 -3 38.01 1.56 -3 -4 3 37.57 1.72 3 4 3 38.32 1.56 4 -4 3 99.72 3.64 4 -4 3 97.29 4.13 4 4 -3 98.59 3.58 -4 -4 -3 99.12 3.97 -4 -4 3 92.51 3.93 4 4 3 89.56 3.56 4 -4 -3 88.87 4.12 4 -4 -3 91.59 3.55 5 -4 3 28.10 1.28 5 -4 3 27.58 1.36 5 4 -3 27.59 1.14 5 -4 3 28.18 1.22 5 -4 -3 28.93 1.37 5 4 3 28.69 1.12 6 -4 3 54.50 2.24 6 -4 3 55.99 2.36 6 -4 3 54.93 1.84 6 -4 3 54.60 1.80 6 4 -3 53.56 2.12 7 4 -3 6.85 0.40 7 -4 3 6.71 0.49 7 -4 3 7.29 0.37 7 -4 3 7.21 0.43 7 -4 3 6.85 0.41 7 4 -3 6.76 0.40 7 -4 3 6.26 0.47 7 -4 -3 8.12 0.44 7 4 3 7.64 0.39 7 4 3 7.92 0.44 7 -4 -3 8.07 0.38 8 -4 3 19.19 1.03 8 -4 3 21.17 0.80 8 -4 3 19.83 0.86 8 4 -3 19.77 0.88 8 -4 3 20.07 0.91 8 4 -3 21.04 0.88 8 4 3 21.49 0.88 8 4 3 21.93 0.91 8 -4 -3 21.35 0.89 8 -4 -3 21.42 0.86 9 4 -3 7.50 0.40 9 4 -3 7.11 0.38 9 -4 3 7.62 0.42 9 -4 3 6.97 0.36 9 4 3 8.00 0.38 9 -4 -3 7.90 0.35 9 4 3 8.14 0.42 9 -4 -3 7.44 0.40 0 -5 -3 61.30 2.52 0 -5 3 62.86 2.33 0 -5 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0.29 9 5 -3 5.24 0.31 9 5 -3 5.29 0.31 9 5 3 5.94 0.31 9 -5 -3 6.13 0.27 9 5 3 6.08 0.34 0 -6 3 6.69 0.36 0 -6 -3 6.28 0.37 1 6 -3 109.57 4.19 -1 -6 -3 110.73 4.67 1 -6 3 113.01 4.33 1 -6 3 115.13 4.28 -1 -6 3 116.32 4.31 1 -6 -3 114.86 4.31 -1 -6 3 112.45 4.66 1 6 3 116.92 4.31 2 -6 3 0.30 0.07 2 6 -3 0.43 0.09 -2 -6 -3 0.32 0.09 2 6 -3 0.20 0.08 -2 -6 3 0.14 0.07 2 6 3 0.13 0.07 2 -6 -3 0.11 0.07 3 -6 3 1.66 0.12 3 -6 3 1.52 0.20 3 6 -3 1.90 0.18 3 6 -3 1.53 0.15 3 6 3 1.29 0.13 3 -6 -3 1.37 0.15 3 6 3 1.13 0.16 4 6 -3 8.78 0.45 4 -6 3 8.20 0.50 4 6 -3 8.33 0.39 4 6 3 7.56 0.43 4 -6 -3 7.55 0.40 5 -6 3 7.30 0.37 5 6 -3 6.57 0.38 5 -6 3 6.83 0.36 5 -6 3 6.86 0.47 5 6 3 6.36 0.38 5 -6 -3 6.22 0.37 6 -6 3 5.52 0.34 6 -6 3 5.33 0.29 6 -6 3 4.91 0.41 6 -6 3 5.48 0.34 6 -6 3 5.51 0.33 6 -6 3 5.30 0.35 6 -6 -3 6.01 0.33 6 6 3 5.85 0.39 7 -6 3 1.33 0.18 7 -6 3 1.37 0.17 7 -6 3 1.48 0.20 7 -6 3 1.19 0.11 7 -6 3 1.25 0.19 7 6 3 0.96 0.14 7 6 3 1.17 0.19 7 -6 -3 1.26 0.15 8 -6 3 1.99 0.19 8 -6 3 1.96 0.11 8 -6 3 1.83 0.19 8 -6 -3 1.82 0.15 8 6 3 2.12 0.21 8 6 3 1.66 0.18 9 6 3 4.40 0.27 9 -6 -3 4.31 0.21 9 6 3 4.42 0.25 0 -7 3 81.68 3.15 0 -7 -3 81.37 3.17 1 -7 3 32.86 1.45 1 7 -3 34.03 1.37 1 -7 3 34.62 1.40 1 -7 -3 34.83 1.43 -1 -7 3 35.40 1.43 2 -7 3 0.99 0.18 2 -7 3 1.00 0.13 2 7 -3 1.29 0.15 2 7 3 1.04 0.13 2 -7 -3 1.07 0.15 2 7 3 1.16 0.16 3 7 -3 2.81 0.24 3 7 -3 2.46 0.21 3 -7 3 2.12 0.25 3 -7 3 2.55 0.19 3 7 3 2.87 0.20 3 7 3 2.92 0.25 3 7 3 2.98 0.25 3 -7 -3 3.28 0.23 4 7 -3 22.52 0.92 4 -7 3 22.68 0.86 4 -7 3 22.70 0.86 4 7 -3 22.41 1.00 4 -7 3 21.69 1.06 4 -7 -3 22.00 0.88 4 7 3 22.37 1.00 4 -7 -3 22.40 0.95 5 -7 3 12.76 0.57 5 -7 3 13.51 0.58 5 7 -3 12.86 0.64 5 -7 3 11.79 0.70 5 7 3 12.26 0.63 5 -7 -3 13.03 0.59 6 -7 3 2.71 0.19 6 -7 3 2.81 0.24 6 -7 3 3.01 0.25 6 -7 3 2.61 0.24 7 -7 3 7.14 0.38 7 -7 3 7.51 0.40 7 -7 3 7.29 0.34 7 7 3 7.24 0.44 7 -7 -3 7.77 0.38 8 -7 3 1.60 0.16 8 -7 3 1.55 0.10 8 -7 -3 1.60 0.13 8 7 3 1.48 0.18 0 -8 3 57.60 2.28 0 -8 -3 56.01 2.29 1 -8 3 86.90 3.35 1 -8 3 86.50 3.30 1 8 -3 88.35 3.24 -1 -8 3 81.75 3.32 1 8 3 83.47 3.21 1 -8 -3 83.27 3.32 2 -8 3 44.60 1.92 2 8 -3 46.19 1.82 2 -8 3 42.46 1.56 2 -8 3 45.77 1.83 2 8 3 46.14 1.89 2 -8 -3 46.91 1.87 2 8 3 46.45 1.89 2 8 3 47.58 1.81 3 -8 3 30.80 1.16 3 8 -3 32.93 1.33 3 8 -3 30.30 1.37 3 -8 3 31.40 1.43 3 -8 3 30.60 1.15 3 8 3 32.24 1.38 3 8 3 34.39 1.29 3 -8 -3 33.99 1.36 3 -8 -3 32.26 1.18 4 8 -3 32.46 1.38 4 -8 3 32.20 1.44 4 -8 3 32.73 1.17 4 -8 3 32.51 1.16 4 8 3 31.56 1.38 4 -8 -3 29.92 1.18 5 -8 3 15.61 0.67 5 -8 3 15.19 0.70 5 -8 3 15.16 0.71 5 -8 3 16.16 0.68 5 -8 -3 16.21 0.72 5 -8 -3 16.80 0.70 5 8 3 16.46 0.76 6 -8 3 44.08 1.62 6 -8 3 44.40 1.56 6 -8 3 42.14 1.44 6 -8 3 44.36 1.49 6 -8 -3 39.29 1.64 6 -8 -3 39.52 1.47 6 8 3 38.41 1.62 7 -8 3 10.56 0.47 7 -8 3 11.42 0.47 7 -8 3 10.98 0.50 7 -8 -3 10.55 0.49 7 8 3 9.94 0.53 8 -8 3 7.91 0.29 8 8 3 6.27 0.36 8 -8 -3 6.89 0.32 0 -9 3 1.33 0.21 0 -9 -3 1.20 0.20 0 -9 3 1.23 0.19 0 -9 3 1.16 0.16 1 9 -3 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5.18 0.30 4 0 -4 5.74 0.36 4 0 -4 5.46 0.27 4 0 4 5.49 0.33 5 0 -4 188.01 7.41 5 0 4 169.47 6.44 5 0 -4 163.24 6.36 5 0 4 164.85 7.35 6 0 4 4.83 0.34 6 0 4 5.05 0.37 6 0 4 5.46 0.37 6 0 -4 4.73 0.39 7 0 4 69.59 2.90 7 0 4 66.60 2.74 7 0 4 69.43 2.21 8 0 4 1.51 0.10 8 0 -4 1.82 0.20 8 0 4 1.51 0.24 8 0 4 1.81 0.21 8 0 4 1.67 0.18 8 0 4 1.54 0.17 8 0 -4 1.58 0.15 9 0 -4 41.46 1.61 9 0 4 43.92 1.61 9 0 -4 42.22 1.64 10 0 4 0.97 0.12 10 0 -4 0.93 0.12 10 0 -4 0.95 0.10 0 -1 4 192.58 7.66 0 1 4 188.85 7.66 1 -1 4 125.59 5.16 -1 1 4 128.33 5.16 -1 -1 4 133.20 5.16 1 1 4 124.82 5.44 -2 -1 -4 272.14 11.07 2 -1 4 264.68 11.64 -2 1 4 274.89 11.03 2 1 4 280.56 11.64 -2 -1 4 283.20 11.05 3 1 -4 28.05 1.15 3 1 -4 28.39 1.35 3 -1 4 26.57 1.16 -3 -1 -4 27.55 1.28 3 -1 4 27.79 1.33 3 -1 -4 31.11 1.37 3 1 4 31.76 1.07 3 1 4 31.68 1.33 3 1 4 30.67 1.18 3 1 4 29.08 1.12 -3 -1 4 31.04 1.26 3 -1 -4 30.74 1.15 4 -1 4 142.78 5.78 4 1 -4 144.23 5.80 4 -1 4 135.42 5.05 4 1 -4 137.33 5.00 4 -1 -4 127.29 5.00 4 1 4 131.49 5.05 4 1 4 133.94 5.76 -4 -1 4 128.29 5.46 4 -1 -4 128.50 5.80 5 -1 4 3.56 0.24 5 1 -4 3.39 0.19 5 -1 4 3.19 0.26 5 -1 -4 2.64 0.17 5 1 4 2.59 0.22 5 1 4 3.05 0.23 5 1 4 2.56 0.23 5 -1 -4 2.62 0.26 6 1 -4 44.05 2.26 6 -1 4 45.87 2.11 6 -1 4 46.97 1.99 6 -1 4 46.06 2.26 6 1 4 50.87 2.25 6 1 4 53.76 2.12 6 1 4 54.02 2.02 6 -1 -4 53.17 2.32 7 -1 4 39.89 1.35 7 -1 4 39.93 1.69 7 -1 4 41.00 1.79 7 1 4 40.03 1.35 7 1 4 40.46 1.77 7 1 4 38.94 1.69 8 1 -4 25.54 0.99 8 1 -4 25.63 1.01 8 -1 4 25.38 1.19 8 -1 4 26.03 0.89 8 -1 4 25.26 0.99 8 -1 4 25.19 0.98 8 -1 4 23.51 1.04 8 -1 -4 22.65 0.98 8 -1 -4 23.41 1.00 8 1 4 22.60 0.99 8 1 4 21.99 0.93 8 1 4 21.68 1.14 9 -1 4 6.83 0.35 9 -1 4 6.71 0.38 9 1 -4 6.75 0.36 9 1 -4 6.83 0.39 9 1 4 7.66 0.41 9 -1 -4 7.75 0.40 9 -1 -4 7.81 0.36 10 1 -4 7.21 0.33 10 1 -4 6.95 0.35 10 -1 4 6.56 0.35 10 -1 -4 7.80 0.33 10 1 4 7.40 0.36 10 -1 -4 6.98 0.35 0 -2 4 114.98 4.64 1 -2 4 143.68 6.64 1 -2 4 152.61 6.28 -1 2 4 153.02 6.28 -1 -2 -4 166.26 6.33 -1 -2 4 165.59 6.30 2 -2 4 120.78 4.94 2 2 -4 113.62 4.29 -2 -2 -4 122.92 4.71 2 -2 -4 109.74 4.30 2 2 4 117.42 4.92 2 -2 -4 109.29 4.94 2 2 4 113.64 4.29 -2 -2 4 114.80 4.68 3 2 -4 82.39 3.48 3 2 -4 81.25 3.02 -3 -2 -4 79.76 3.32 3 -2 4 80.20 3.04 3 -2 4 82.75 3.48 3 2 4 80.69 2.76 3 2 4 78.45 3.04 3 2 4 82.92 3.46 3 -2 -4 77.12 3.02 3 -2 -4 79.02 3.49 3 2 4 78.09 3.00 -3 -2 4 80.15 3.30 4 2 -4 2.40 0.15 4 -2 4 2.37 0.20 -4 -2 -4 2.07 0.19 4 -2 4 2.47 0.18 4 2 4 1.97 0.17 4 2 4 1.69 0.11 -4 -2 4 1.88 0.17 4 -2 -4 1.96 0.21 4 2 4 1.92 0.17 4 -2 -4 1.98 0.15 5 2 -4 204.37 8.65 5 2 -4 196.28 7.48 5 -2 4 201.86 8.04 5 -2 4 207.53 7.57 5 -2 4 201.30 8.65 5 2 4 198.62 7.55 5 -2 -4 201.69 8.68 6 -2 4 7.28 0.48 6 2 -4 6.73 0.35 6 -2 4 7.29 0.43 6 -2 4 7.78 0.47 6 2 4 7.40 0.44 6 -2 -4 6.92 0.51 7 -2 4 8.95 0.54 7 -2 4 9.05 0.41 7 -2 4 9.12 0.56 7 -2 4 8.45 0.44 7 2 4 8.33 0.46 8 -2 4 2.49 0.24 8 -2 4 2.35 0.22 8 2 -4 2.34 0.19 8 -2 4 2.67 0.21 8 2 -4 2.42 0.22 8 -2 4 2.41 0.29 8 -2 4 2.41 0.25 8 2 4 2.63 0.17 8 2 4 2.59 0.23 8 -2 -4 2.41 0.24 8 2 4 2.58 0.23 8 -2 -4 2.46 0.19 9 2 -4 1.53 0.14 9 -2 4 1.70 0.17 9 -2 4 1.61 0.20 9 2 -4 1.59 0.17 9 -2 4 1.65 0.16 9 2 4 1.50 0.13 9 -2 -4 1.30 0.17 9 2 4 1.36 0.17 9 2 4 1.47 0.17 9 -2 -4 1.45 0.14 10 2 -4 1.27 0.11 10 2 -4 1.27 0.13 10 2 4 1.11 0.14 10 -2 -4 1.35 0.10 10 -2 -4 1.08 0.13 10 2 4 1.27 0.14 0 -3 4 5.60 0.29 0 -3 -4 6.43 0.33 0 -3 4 6.03 0.31 1 -3 4 42.28 1.68 1 -3 4 42.20 1.82 -1 -3 -4 43.53 1.86 1 -3 4 37.38 1.93 -1 -3 4 47.32 1.85 1 -3 -4 46.54 1.72 1 -3 -4 47.69 1.84 1 3 4 47.47 1.71 2 -3 4 21.44 0.89 2 -3 4 21.39 1.00 2 -3 4 21.18 0.84 2 3 -4 20.85 0.87 -2 -3 -4 21.87 0.98 2 3 4 21.96 0.88 2 3 4 21.06 0.80 2 -3 -4 22.77 1.01 2 -3 -4 21.64 0.88 3 3 -4 15.68 0.62 3 -3 4 14.74 0.72 -3 -3 -4 14.82 0.71 3 -3 4 14.96 0.65 3 3 -4 14.42 0.59 3 -3 -4 13.72 0.62 3 -3 -4 13.66 0.72 3 3 4 14.19 0.61 3 3 4 13.74 0.58 -3 -3 4 13.56 0.68 4 3 -4 11.00 0.49 4 -3 4 11.18 0.53 4 -3 4 10.24 0.55 4 -3 4 10.75 0.59 -4 -3 -4 10.43 0.58 -4 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0 -4 -4 84.94 3.37 0 4 4 80.91 3.11 0 -4 -4 79.51 3.12 1 -4 4 220.57 8.46 -1 -4 -4 236.38 9.20 1 -4 4 228.43 8.42 1 4 4 225.65 8.44 -1 -4 4 235.21 9.18 1 -4 -4 218.86 8.45 -2 -4 -4 59.85 2.43 2 -4 4 57.85 2.23 2 -4 4 58.48 2.17 2 4 -4 59.68 2.21 2 4 -4 55.75 2.16 2 -4 4 57.28 2.52 -2 -4 4 57.10 2.40 2 -4 -4 55.80 2.21 2 4 4 58.20 2.22 2 4 4 54.70 2.00 -3 -4 -4 12.46 0.63 3 4 -4 11.52 0.50 3 -4 4 12.33 0.57 3 -4 4 11.47 0.62 3 4 -4 11.87 0.53 3 -4 -4 12.46 0.54 -3 -4 4 11.19 0.59 3 4 4 11.68 0.54 4 -4 4 1.66 0.18 4 4 -4 1.46 0.12 4 -4 4 1.68 0.19 4 -4 4 1.32 0.18 -4 -4 -4 1.58 0.19 4 4 -4 1.33 0.14 4 4 4 2.03 0.15 4 4 4 1.93 0.15 -4 -4 4 1.87 0.19 4 -4 -4 1.91 0.20 4 -4 -4 1.90 0.15 5 4 -4 75.65 2.86 5 -4 4 76.11 2.94 5 -4 4 72.39 3.32 5 -4 4 74.39 3.10 5 -4 -4 72.87 3.33 5 4 4 75.87 2.82 6 -4 4 16.99 0.68 6 -4 4 16.96 0.84 6 4 -4 15.98 0.73 6 -4 4 17.15 0.87 6 -4 4 17.37 0.66 7 4 -4 14.80 0.66 7 -4 4 14.43 0.66 7 -4 4 14.84 0.80 7 -4 4 14.51 0.59 7 -4 4 15.20 0.70 7 -4 4 13.64 0.75 7 -4 -4 13.60 0.63 7 4 4 13.38 0.64 7 4 4 13.65 0.67 7 -4 -4 13.84 0.67 8 -4 4 3.12 0.23 8 -4 4 2.85 0.33 8 -4 4 3.03 0.26 8 4 -4 3.18 0.23 8 4 -4 2.84 0.24 8 -4 4 3.33 0.27 8 -4 -4 3.18 0.27 8 4 4 3.07 0.22 8 -4 -4 3.10 0.21 8 4 4 3.27 0.27 9 -4 4 1.84 0.20 9 -4 4 1.71 0.17 9 -4 4 1.74 0.19 9 4 -4 1.67 0.16 9 4 -4 1.62 0.17 9 -4 -4 1.98 0.19 9 4 4 1.95 0.16 9 -4 -4 1.98 0.15 9 4 4 2.03 0.19 0 -5 -4 170.13 6.32 0 -5 4 174.40 6.29 0 -5 -4 166.20 6.84 0 -5 -4 164.00 6.16 -1 -5 -4 12.62 0.57 1 -5 4 14.26 0.56 -1 -5 -4 14.14 0.63 1 -5 4 14.20 0.60 1 -5 -4 11.12 0.54 1 5 4 11.79 0.57 -1 -5 4 11.31 0.60 -1 -5 4 11.43 0.56 1 -5 -4 11.65 0.57 2 -5 4 187.61 7.03 -2 -5 -4 185.54 7.63 2 5 -4 177.79 6.82 2 5 -4 187.94 6.99 2 -5 4 189.79 6.95 2 5 4 193.22 7.00 2 -5 -4 193.93 7.00 -2 -5 4 183.13 7.61 3 -5 4 8.65 0.48 -3 -5 -4 8.71 0.52 3 5 -4 8.22 0.41 3 5 -4 8.81 0.45 -3 -5 4 9.64 0.51 3 -5 -4 10.17 0.46 3 5 4 9.70 0.46 4 -5 4 77.53 3.14 4 5 -4 75.97 3.07 4 5 -4 76.61 2.97 4 5 4 84.33 3.08 4 5 4 84.08 3.08 4 -5 -4 82.81 3.06 5 -5 4 6.24 0.33 5 5 -4 6.03 0.35 5 -5 4 6.09 0.42 5 5 4 6.47 0.35 6 5 -4 79.74 3.11 6 -5 4 80.97 3.24 6 -5 4 83.68 2.66 6 -5 4 79.61 2.59 7 -5 4 4.54 0.32 7 -5 4 4.32 0.22 7 -5 4 4.34 0.28 7 -5 4 4.17 0.31 7 -5 -4 4.71 0.34 7 5 4 4.60 0.35 7 5 4 4.52 0.28 7 -5 -4 4.76 0.28 8 -5 4 17.18 0.76 8 -5 4 17.27 0.68 8 -5 4 16.80 0.73 8 5 4 17.25 0.74 8 5 4 16.49 0.77 8 -5 -4 16.20 0.74 8 -5 -4 17.19 0.72 9 -5 4 3.76 0.24 9 -5 4 3.16 0.22 9 5 -4 3.41 0.23 9 5 -4 2.73 0.22 9 -5 -4 3.40 0.24 9 -5 -4 3.53 0.19 9 5 4 3.60 0.24 9 5 4 3.20 0.21 0 -6 4 5.80 0.33 0 -6 -4 5.83 0.32 0 -6 -4 5.65 0.35 1 -6 4 181.99 6.78 -1 -6 -4 177.54 6.61 1 -6 4 183.62 6.72 -1 -6 -4 179.76 7.34 1 6 -4 179.88 6.59 -1 -6 4 180.72 6.75 1 6 4 180.47 6.75 1 -6 -4 182.38 6.76 -1 -6 4 174.29 7.32 -2 -6 -4 50.13 2.18 2 -6 4 51.50 1.95 2 6 -4 50.75 1.93 2 -6 4 51.68 2.04 2 6 4 52.33 2.01 2 6 4 48.14 1.93 2 -6 -4 51.60 2.00 -2 -6 4 47.47 2.16 3 6 -4 194.62 6.95 3 -6 4 197.33 7.19 3 6 -4 194.27 7.12 3 6 4 177.50 6.91 3 -6 -4 191.89 7.11 3 6 4 184.50 7.12 4 6 -4 10.83 0.49 4 6 -4 10.84 0.53 4 -6 4 10.50 0.47 4 -6 4 10.80 0.60 4 6 4 9.91 0.53 4 -6 -4 9.85 0.50 5 6 -4 14.37 0.67 5 -6 4 14.11 0.59 5 -6 4 14.29 0.59 5 -6 4 14.29 0.76 5 6 4 12.68 0.65 6 -6 4 20.36 0.77 6 -6 4 19.69 0.84 6 -6 4 19.04 0.82 6 -6 4 18.46 0.77 6 -6 4 17.03 0.93 6 -6 4 20.01 0.76 6 -6 -4 18.40 0.82 6 -6 -4 18.04 0.84 6 6 4 19.16 0.88 7 -6 4 36.19 1.42 7 -6 4 36.12 1.25 7 -6 4 35.55 1.36 7 -6 4 35.64 1.36 7 6 4 35.70 1.44 7 -6 -4 36.47 1.43 7 -6 -4 33.99 1.40 7 6 4 36.34 1.45 8 -6 4 5.61 0.34 8 -6 4 5.98 0.33 8 -6 4 5.94 0.32 8 6 4 5.69 0.33 8 -6 -4 5.71 0.35 8 6 4 5.78 0.36 8 -6 -4 5.98 0.31 9 6 4 14.03 0.61 9 6 4 14.46 0.61 0 -7 4 26.13 1.10 0 -7 -4 25.66 1.13 1 -7 4 34.36 1.52 1 7 -4 36.36 1.45 1 -7 4 34.72 1.46 -1 -7 4 37.56 1.50 1 -7 -4 37.74 1.51 2 7 -4 97.01 3.51 2 -7 4 96.37 3.66 2 -7 4 95.20 3.55 2 -7 -4 92.68 3.60 2 7 4 89.66 3.49 2 7 4 89.40 3.60 3 -7 4 10.06 0.58 3 7 -4 10.53 0.50 3 -7 4 9.58 0.45 3 7 -4 10.18 0.54 3 7 4 10.30 0.55 3 7 4 10.07 0.47 3 -7 -4 9.88 0.52 3 7 4 10.29 0.55 4 -7 4 71.18 2.34 4 7 -4 69.81 2.71 4 -7 4 68.96 2.89 4 -7 4 71.06 2.37 4 7 -4 68.19 2.81 4 7 4 76.92 2.83 4 -7 -4 71.87 2.40 4 -7 -4 75.99 2.78 5 -7 4 0.59 0.18 5 -7 4 0.56 0.10 5 -7 4 0.65 0.13 5 -7 4 0.80 0.15 5 -7 4 0.59 0.14 5 -7 -4 1.05 0.17 5 -7 -4 0.82 0.14 5 7 4 0.97 0.19 6 -7 4 33.81 1.29 6 -7 4 33.83 1.18 6 -7 4 34.57 1.21 6 -7 4 32.61 1.27 6 -7 -4 30.91 1.32 6 7 4 30.88 1.34 7 -7 4 5.32 0.33 7 -7 4 5.63 0.28 7 -7 4 5.82 0.35 7 -7 4 5.20 0.32 7 7 4 5.76 0.38 7 -7 -4 6.09 0.32 8 -7 4 33.68 1.18 8 -7 4 35.47 1.33 8 7 4 33.25 1.37 8 7 4 33.93 1.34 8 -7 -4 36.50 1.34 0 -8 4 0.93 0.16 0 -8 4 0.88 0.17 0 -8 -4 1.02 0.19 1 8 -4 44.76 1.73 1 -8 4 44.09 1.82 1 -8 4 44.44 1.76 1 -8 -4 41.32 1.78 -1 -8 4 40.73 1.78 2 8 -4 3.33 0.26 2 -8 4 3.29 0.32 2 -8 4 3.42 0.25 2 8 4 4.05 0.26 2 -8 -4 3.42 0.28 2 8 4 3.36 0.29 3 -8 4 11.34 0.69 3 8 -4 12.20 0.61 3 8 -4 11.31 0.64 3 -8 4 11.62 0.54 3 -8 4 12.82 0.56 3 8 4 12.96 0.66 3 -8 -4 13.54 0.63 3 8 4 13.23 0.66 3 -8 -4 13.13 0.58 3 8 4 13.43 0.59 4 -8 4 5.49 0.39 4 -8 4 5.49 0.45 4 -8 4 5.66 0.36 4 -8 4 6.36 0.36 4 -8 4 6.47 0.37 4 8 -4 5.91 0.42 4 8 -4 5.97 0.36 4 -8 -4 7.69 0.40 4 -8 -4 7.39 0.38 4 8 4 7.73 0.42 4 8 4 7.37 0.43 5 -8 4 15.98 0.66 5 -8 4 15.63 0.65 5 -8 4 15.85 0.70 5 -8 4 15.21 0.66 5 -8 -4 14.26 0.69 5 8 4 14.13 0.72 5 -8 -4 13.88 0.65 6 -8 4 1.46 0.18 6 -8 4 1.58 0.19 6 -8 4 1.26 0.19 6 -8 4 1.23 0.12 6 8 4 1.12 0.19 6 -8 -4 1.23 0.15 7 -8 4 1.12 0.10 7 -8 4 1.07 0.14 7 -8 4 1.15 0.16 7 8 4 0.96 0.16 7 -8 -4 0.89 0.12 8 8 4 0.58 0.11 8 -8 -4 0.64 0.08 0 9 4 58.03 2.21 0 -9 4 65.58 2.56 0 -9 4 64.28 2.53 0 -9 -4 60.48 2.54 0 -9 4 65.52 2.07 1 9 -4 32.60 1.35 1 -9 4 32.74 1.42 1 -9 4 31.99 1.14 1 -9 4 31.49 1.36 -1 -9 4 31.25 1.13 1 9 4 32.16 1.31 -1 -9 4 30.50 1.39 1 9 4 31.32 1.23 1 -9 -4 32.03 1.39 2 -9 4 15.15 0.69 2 -9 4 14.82 0.62 2 9 -4 15.40 0.71 2 -9 4 14.80 0.79 2 9 4 13.37 0.73 2 9 4 13.16 0.73 2 -9 -4 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0 17 13.84 0.63 2 0 17 0.42 0.11 3 0 17 1.64 0.18 3 0 17 1.49 0.17 4 0 17 1.44 0.17 4 0 17 1.66 0.17 5 0 17 0.51 0.09 5 0 17 0.51 0.10 0 -1 17 11.51 0.54 0 1 17 11.60 0.55 0 1 17 11.51 0.56 1 -1 17 2.07 0.21 -1 1 17 1.85 0.19 1 1 17 1.49 0.20 1 1 17 1.48 0.19 -2 1 17 0.53 0.12 2 -1 17 0.43 0.12 2 1 17 0.74 0.14 2 1 17 0.57 0.12 3 -1 17 5.53 0.35 3 1 17 6.33 0.35 -3 -1 17 6.39 0.38 3 1 17 6.57 0.37 4 -1 17 4.97 0.30 4 1 17 5.34 0.31 -4 -1 17 5.55 0.33 4 1 17 5.56 0.32 5 -1 17 5.69 0.28 5 1 17 4.78 0.27 -5 -1 17 4.71 0.29 5 1 17 4.92 0.28 0 2 17 25.25 0.99 0 -2 17 25.40 0.99 0 2 17 26.81 1.05 0 -2 17 24.46 1.07 1 -2 17 6.71 0.38 -1 2 17 6.84 0.38 -1 -2 17 6.09 0.39 -1 -2 17 6.47 0.37 1 2 17 6.54 0.37 1 2 17 6.34 0.38 2 -2 17 1.59 0.19 2 2 17 1.47 0.18 2 2 17 1.54 0.18 -2 -2 17 1.42 0.19 3 -2 17 17.89 0.73 3 2 17 18.10 0.77 3 2 17 16.97 0.72 -3 -2 17 18.06 0.80 4 -2 17 6.71 0.36 4 -2 17 6.53 0.36 4 2 17 7.09 0.36 -4 -2 17 7.57 0.40 4 2 17 7.48 0.38 5 -2 17 5.88 0.29 -5 -2 17 5.17 0.31 0 3 17 9.01 0.45 0 3 17 8.94 0.46 0 -3 17 9.18 0.46 0 -3 17 8.42 0.48 1 -3 17 0.52 0.12 -1 3 17 0.67 0.13 1 -3 17 0.41 0.12 -1 -3 17 0.56 0.14 1 3 17 0.47 0.12 -1 -3 17 0.33 0.11 1 3 17 0.40 0.11 2 -3 17 19.46 0.80 2 -3 17 19.48 0.87 -2 3 17 19.89 0.83 2 3 17 20.01 0.84 2 3 17 20.67 0.80 -2 -3 17 19.87 0.88 3 -3 17 14.21 0.63 3 -3 17 14.41 0.68 3 3 17 15.48 0.67 3 3 17 15.81 0.64 -3 -3 17 16.04 0.72 4 -3 17 7.42 0.37 4 -3 17 6.90 0.39 -4 -3 17 8.06 0.42 4 3 17 7.61 0.39 4 3 17 7.71 0.37 5 -3 17 2.65 0.17 -5 -3 17 2.49 0.20 5 3 17 2.85 0.19 0 -4 17 0.50 0.13 0 4 17 0.45 0.11 0 4 17 0.48 0.11 0 -4 17 0.47 0.12 -1 4 17 24.20 0.98 1 -4 17 23.94 1.04 1 -4 17 23.50 0.94 1 4 17 24.20 0.94 -1 -4 17 25.44 1.05 -1 -4 17 24.80 0.94 1 4 17 25.16 0.99 2 -4 17 10.26 0.52 2 -4 17 10.48 0.48 -2 4 17 10.64 0.49 2 4 17 9.75 0.47 2 4 17 9.87 0.48 -2 -4 17 9.88 0.52 3 -4 17 9.54 0.42 3 -4 17 9.23 0.45 3 4 17 7.65 0.40 -3 -4 17 8.02 0.45 3 4 17 7.22 0.39 4 -4 17 6.77 0.33 4 -4 17 6.66 0.35 -4 -4 17 6.14 0.36 4 4 17 6.80 0.34 4 4 17 6.24 0.32 5 -4 17 14.20 0.59 -5 -4 17 14.40 0.62 0 -5 17 5.17 0.31 0 5 17 5.08 0.30 0 -5 17 5.14 0.33 0 5 17 5.04 0.30 -1 5 17 3.62 0.24 1 -5 17 3.61 0.27 1 -5 17 3.92 0.26 1 5 17 2.99 0.23 -1 -5 17 3.23 0.26 -1 -5 17 3.22 0.24 1 5 17 3.24 0.23 2 -5 17 2.16 0.19 2 -5 17 2.08 0.20 -2 5 17 2.01 0.17 -2 -5 17 1.59 0.19 2 5 17 1.35 0.16 2 5 17 1.52 0.17 -3 5 17 2.84 0.20 3 -5 17 2.35 0.19 3 -5 17 2.87 0.22 3 5 17 2.79 0.19 3 5 17 2.78 0.20 -3 -5 17 3.10 0.23 4 -5 17 5.87 0.30 4 -5 17 5.96 0.32 -4 5 17 6.03 0.30 4 5 17 6.10 0.30 -4 -5 17 6.15 0.33 0 6 17 0.58 0.11 0 -6 17 0.55 0.12 0 -6 17 0.54 0.12 -1 6 17 2.31 0.18 1 -6 17 2.53 0.21 1 -6 17 1.92 0.19 -1 -6 17 2.19 0.19 1 6 17 2.46 0.18 -1 -6 17 2.53 0.21 1 6 17 2.07 0.19 2 -6 17 6.12 0.33 2 -6 17 7.50 0.38 -2 6 17 7.39 0.35 2 6 17 6.33 0.34 2 6 17 6.98 0.34 -2 -6 17 7.18 0.38 -3 6 17 0.58 0.09 3 -6 17 0.69 0.11 3 6 17 0.61 0.09 3 6 17 0.46 0.09 -3 -6 17 0.53 0.10 0 -7 17 0.53 0.10 0 -7 17 0.58 0.11 0 7 17 0.56 0.09 -1 7 17 3.34 0.20 1 -7 17 3.61 0.23 1 -7 17 3.27 0.22 -1 -7 17 3.22 0.22 2 -7 17 2.79 0.20 -2 -7 17 3.16 0.21 0 0 18 0.28 0.11 1 0 18 0.08 0.09 2 0 18 45.29 1.59 3 0 18 0.15 0.08 4 0 18 6.76 0.33 0 -1 18 1.82 0.20 0 1 18 1.90 0.19 0 1 18 1.80 0.19 -1 1 18 14.01 0.64 1 -1 18 15.01 0.64 1 1 18 14.72 0.65 1 1 18 14.31 0.62 2 -1 18 3.83 0.27 -2 1 18 4.12 0.26 2 1 18 3.92 0.26 2 1 18 3.84 0.26 3 -1 18 8.88 0.42 -3 1 18 9.25 0.42 3 1 18 7.97 0.41 3 1 18 8.30 0.41 4 -1 18 9.06 0.41 4 1 18 9.23 0.41 4 1 18 9.75 0.44 0 2 18 8.18 0.42 0 -2 18 8.49 0.43 0 2 18 8.71 0.43 -1 2 18 8.43 0.43 1 -2 18 8.66 0.43 -1 -2 18 8.39 0.44 1 2 18 8.87 0.44 1 2 18 8.24 0.42 -1 -2 18 8.35 0.42 2 -2 18 3.38 0.25 -2 2 18 3.79 0.25 2 2 18 3.70 0.26 -2 -2 18 3.36 0.25 2 2 18 3.59 0.25 3 -2 18 1.75 0.18 -3 2 18 2.13 0.17 3 2 18 2.41 0.19 -3 -2 18 2.23 0.20 3 2 18 2.17 0.18 -4 2 18 1.32 0.13 4 -2 18 1.27 0.15 -4 -2 18 1.41 0.15 4 2 18 1.36 0.14 4 2 18 1.39 0.14 0 -3 18 0.82 0.14 0 -3 18 0.58 0.12 0 3 18 0.75 0.13 0 3 18 0.81 0.13 1 -3 18 0.98 0.15 -1 3 18 1.01 0.14 1 -3 18 0.99 0.16 -1 -3 18 0.95 0.14 1 3 18 0.94 0.14 1 3 18 0.95 0.14 -1 -3 18 1.08 0.16 -2 3 18 5.82 0.31 2 -3 18 4.95 0.31 2 -3 18 4.84 0.30 -2 -3 18 5.53 0.33 2 3 18 5.95 0.32 2 3 18 4.90 0.29 -3 3 18 1.16 0.13 3 -3 18 0.92 0.14 -3 -3 18 1.22 0.15 3 3 18 1.06 0.14 3 3 18 1.20 0.13 4 -3 18 11.79 0.52 -4 3 18 12.84 0.51 4 3 18 11.85 0.51 -4 -3 18 11.71 0.53 0 -4 18 17.26 0.71 0 4 18 18.51 0.74 0 4 18 17.77 0.71 0 -4 18 18.20 0.79 1 -4 18 5.07 0.31 1 -4 18 4.75 0.29 -1 4 18 4.92 0.29 1 4 18 4.87 0.29 -1 -4 18 4.89 0.29 -1 -4 18 5.21 0.32 1 4 18 5.33 0.29 -2 4 18 0.88 0.12 2 -4 18 0.96 0.14 2 -4 18 0.83 0.13 2 4 18 0.85 0.12 -2 -4 18 0.93 0.14 2 4 18 0.97 0.14 3 -4 18 1.95 0.17 3 -4 18 1.77 0.16 -3 4 18 1.63 0.15 3 4 18 1.80 0.15 -3 -4 18 1.97 0.18 3 4 18 1.69 0.16 -4 -4 18 0.60 0.10 0 -5 18 0.20 0.09 0 -5 18 0.22 0.08 0 5 18 0.18 0.07 1 -5 18 6.46 0.32 -1 5 18 6.56 0.32 1 -5 18 6.95 0.36 -1 -5 18 5.66 0.31 1 5 18 5.48 0.31 -1 -5 18 6.06 0.35 1 5 18 5.81 0.31 2 -5 18 1.94 0.17 2 -5 18 1.97 0.17 -2 5 18 2.12 0.16 2 5 18 2.07 0.17 -2 -5 18 2.15 0.18 2 5 18 2.01 0.16 3 -5 18 0.24 0.07 -3 5 18 0.29 0.07 3 5 18 0.45 0.08 0 -6 18 3.49 0.22 0 6 18 3.69 0.21 0 -6 18 3.66 0.24 1 -6 18 0.14 0.07 1 -6 18 0.09 0.06 -1 6 18 0.11 0.06 1 6 18 0.21 0.07 -1 -6 18 0.28 0.08 2 -6 18 27.77 1.12 -2 -6 18 30.43 1.13 0 0 19 -0.03 0.07 1 0 19 4.16 0.26 2 0 19 0.16 0.08 3 0 19 2.53 0.18 0 1 19 13.22 0.58 0 1 19 13.81 0.57 0 -1 19 13.37 0.57 1 -1 19 3.93 0.26 -1 1 19 4.04 0.25 1 1 19 3.42 0.24 1 1 19 3.80 0.24 2 -1 19 2.01 0.18 2 1 19 2.71 0.19 2 1 19 2.47 0.19 3 -1 19 0.79 0.12 3 1 19 0.49 0.09 3 1 19 0.61 0.10 0 2 19 0.01 0.07 0 -2 19 0.06 0.08 0 2 19 0.05 0.06 -1 2 19 7.64 0.38 1 -2 19 7.55 0.38 1 2 19 7.80 0.37 1 2 19 7.56 0.37 2 -2 19 1.60 0.17 -2 2 19 1.96 0.16 2 2 19 1.96 0.16 2 2 19 2.27 0.17 3 -2 19 6.20 0.30 -3 2 19 6.67 0.31 -3 -2 19 5.98 0.31 3 2 19 5.90 0.30 3 2 19 6.29 0.30 0 -3 19 6.35 0.34 0 3 19 5.99 0.31 0 3 19 6.13 0.33 0 -3 19 6.87 0.33 1 -3 19 8.84 0.42 1 -3 19 9.04 0.44 -1 3 19 9.15 0.43 1 3 19 10.23 0.44 1 3 19 9.18 0.42 -1 -3 19 9.44 0.45 2 -3 19 5.61 0.31 -2 3 19 6.16 0.31 2 3 19 6.40 0.31 -2 -3 19 6.39 0.33 2 3 19 6.06 0.31 -3 -3 19 6.50 0.33 0 -4 19 0.09 0.07 0 4 19 0.02 0.05 0 -4 19 -0.03 0.06 1 -4 19 5.34 0.28 -1 4 19 5.21 0.27 1 -4 19 5.54 0.29 1 4 19 4.72 0.27 1 4 19 5.23 0.27 -1 -4 19 4.91 0.29 2 -4 19 4.31 0.25 -2 4 19 4.65 0.25 -2 -4 19 4.95 0.27 2 4 19 4.48 0.24 0 -5 19 0.76 0.11 1 -5 19 3.15 0.20 -1 -5 19 3.13 0.21 1 0 20 1.51 0.14 1 -1 20 5.38 0.27 1 1 20 4.24 0.25 0 2 20 0.78 0.11 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 44299 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 Br1 Br 0.25039(4) -0.08253(3) -0.05489(2) 0.04120(14) Uani 1 1 d . S1 S 0.56196(8) 0.26452(7) 0.19245(4) 0.02867(18) Uani 1 1 d . O1 O 0.5126(2) 0.31236(19) 0.02529(12) 0.0265(5) Uani 1 1 d . O2 O 0.5345(3) 0.2111(2) 0.26667(13) 0.0370(6) Uani 1 1 d . O3 O 0.7154(2) 0.2938(2) 0.17178(13) 0.0356(6) Uani 1 1 d . N1 N 0.4642(3) 0.3849(2) 0.18790(17) 0.0263(6) Uani 1 1 d . H1N H 0.497(4) 0.420(3) 0.157(2) 0.020(9) Uiso 1 1 d . N2 N 0.3286(3) 0.5112(2) 0.07098(16) 0.0264(6) Uani 1 1 d . C1 C 0.4851(3) 0.1675(3) 0.12190(19) 0.0272(6) Uani 1 1 d . C2 C 0.4461(4) 0.0545(3) 0.1448(2) 0.0325(7) Uani 1 1 d . H2 H 0.464(4) 0.038(4) 0.198(2) 0.034(10) Uiso 1 1 d . C3 C 0.3801(4) -0.0219(3) 0.0921(2) 0.0346(8) Uani 1 1 d . H3 H 0.360(4) -0.100(3) 0.108(2) 0.025(8) Uiso 1 1 d . C4 C 0.3493(4) 0.0181(3) 0.0177(2) 0.0313(7) Uani 1 1 d . C5 C 0.3860(4) 0.1302(3) -0.0073(2) 0.0279(7) Uani 1 1 d . H5 H 0.369(4) 0.152(3) -0.055(2) 0.022(9) Uiso 1 1 d . C6 C 0.4587(3) 0.2047(3) 0.04506(18) 0.0244(6) Uani 1 1 d . C7 C 0.4278(4) 0.3809(3) -0.03104(18) 0.0274(6) Uani 1 1 d . H7A H 0.503(5) 0.446(4) -0.048(2) 0.038(10) Uiso 1 1 d . H7B H 0.405(4) 0.330(3) -0.076(2) 0.028(9) Uiso 1 1 d . C8 C 0.2876(4) 0.4315(3) 0.00749(19) 0.0281(7) Uani 1 1 d . H8A H 0.237(5) 0.472(4) -0.034(3) 0.043(11) Uiso 1 1 d . H8B H 0.229(4) 0.368(3) 0.026(2) 0.025(8) Uiso 1 1 d . C9 C 0.2444(5) 0.4920(3) 0.14306(17) 0.0268(6) Uani 1 1 d . H9A H 0.267(4) 0.552(3) 0.175(2) 0.026(8) Uiso 1 1 d . H9B H 0.138(4) 0.487(3) 0.133(2) 0.023(8) Uiso 1 1 d . C10 C 0.2951(3) 0.3782(3) 0.18300(18) 0.0249(6) Uani 1 1 d . H10 H 0.262(4) 0.310(3) 0.1516(18) 0.018(7) Uiso 1 1 d . C11 C 0.2183(3) 0.3626(3) 0.26252(18) 0.0269(7) Uani 1 1 d . H11A H 0.280(4) 0.314(3) 0.294(2) 0.024(9) Uiso 1 1 d . H11B H 0.214(4) 0.437(3) 0.289(2) 0.029(9) Uiso 1 1 d . C12 C 0.0586(4) 0.3091(3) 0.25510(18) 0.0290(6) Uani 1 1 d . H12 H -0.003(4) 0.350(3) 0.209(2) 0.023(9) Uiso 1 1 d . C13 C 0.0659(4) 0.1794(3) 0.2353(2) 0.0345(7) Uani 1 1 d . H13A H -0.029(5) 0.146(4) 0.230(2) 0.036(11) Uiso 1 1 d . H13B H 0.119(5) 0.134(4) 0.278(3) 0.045(12) Uiso 1 1 d . H13C H 0.114(5) 0.164(4) 0.187(3) 0.054(13) Uiso 1 1 d . C14 C -0.0323(4) 0.3259(4) 0.3297(2) 0.0361(8) Uani 1 1 d . H14A H -0.048(5) 0.398(4) 0.338(3) 0.040(11) Uiso 1 1 d . H14B H -0.127(5) 0.295(4) 0.324(3) 0.042(11) Uiso 1 1 d . H14C H 0.020(5) 0.295(4) 0.373(3) 0.046(12) Uiso 1 1 d . C15 C 0.3254(4) 0.6329(3) 0.0466(2) 0.0358(8) Uani 1 1 d . H15A H 0.2200 0.6564 0.0361 0.036(10) Uiso 1 1 calc R H15B H 0.3863 0.6423 -0.0008 0.031(9) Uiso 1 1 calc R H15C H 0.3675 0.6821 0.0881 0.062(14) Uiso 1 1 calc R 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 0.0434(2) 0.02670(19) 0.0535(2) -0.00909(14) -0.00049(19) -0.00096(17) S1 0.0268(3) 0.0353(4) 0.0238(3) 0.0015(3) -0.0020(3) 0.0058(3) O1 0.0270(10) 0.0265(11) 0.0260(10) 0.0025(9) -0.0002(9) -0.0013(9) O2 0.0420(13) 0.0443(14) 0.0246(11) 0.0064(10) 0.0001(10) 0.0115(11) O3 0.0256(11) 0.0495(14) 0.0317(12) -0.0011(10) -0.0034(9) 0.0044(10) N1 0.0245(13) 0.0298(14) 0.0245(13) 0.0020(12) 0.0005(11) 0.0011(11) N2 0.0297(14) 0.0222(13) 0.0273(14) 0.0004(10) -0.0003(11) -0.0001(10) C1 0.0252(14) 0.0285(16) 0.0278(15) 0.0010(12) 0.0048(12) 0.0076(13) C2 0.0346(16) 0.0309(17) 0.0319(17) 0.0044(13) 0.0068(14) 0.0080(14) C3 0.0352(18) 0.0249(16) 0.044(2) 0.0043(15) 0.0115(15) 0.0040(14) C4 0.0280(15) 0.0244(16) 0.0414(19) -0.0053(14) 0.0027(14) 0.0032(13) C5 0.0260(15) 0.0276(16) 0.0300(17) -0.0010(13) 0.0015(13) 0.0057(13) C6 0.0229(13) 0.0207(14) 0.0296(15) -0.0004(12) 0.0036(11) 0.0041(11) C7 0.0354(16) 0.0258(15) 0.0210(14) 0.0032(12) -0.0018(13) -0.0023(13) C8 0.0323(16) 0.0263(15) 0.0256(15) 0.0024(13) -0.0046(12) -0.0015(13) C9 0.0277(15) 0.0260(14) 0.0268(14) -0.0029(12) 0.0020(15) 0.0019(14) C10 0.0240(14) 0.0267(15) 0.0239(15) -0.0012(12) -0.0010(11) 0.0010(11) C11 0.0256(16) 0.0304(16) 0.0248(15) -0.0027(13) -0.0002(12) 0.0005(13) C12 0.0263(14) 0.0380(17) 0.0227(14) 0.0010(13) 0.0036(13) -0.0002(14) C13 0.0371(19) 0.0350(18) 0.0315(18) -0.0024(15) 0.0032(15) -0.0074(15) C14 0.0321(18) 0.045(2) 0.0312(18) -0.0044(16) 0.0065(15) -0.0015(16) C15 0.0459(19) 0.0265(16) 0.0351(19) 0.0006(14) 0.0027(15) 0.0012(15) 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' S S 0.3331 0.5567 '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 O2 S1 O3 118.53(14) O2 S1 N1 108.38(15) O3 S1 N1 106.66(15) O2 S1 C1 105.98(16) O3 S1 C1 109.59(14) N1 S1 C1 107.22(14) C6 O1 C7 118.4(2) C10 N1 S1 119.1(2) C10 N1 H1N 113(3) S1 N1 H1N 107(3) C15 N2 C9 112.3(3) C15 N2 C8 112.1(3) C9 N2 C8 114.3(3) C2 C1 C6 120.3(3) C2 C1 S1 118.8(3) C6 C1 S1 120.9(2) C3 C2 C1 120.3(3) C3 C2 H2 125(3) C1 C2 H2 115(3) C4 C3 C2 118.4(3) C4 C3 H3 122(2) C2 C3 H3 119(2) C3 C4 C5 123.0(3) C3 C4 Br1 119.5(3) C5 C4 Br1 117.5(3) C4 C5 C6 118.1(3) C4 C5 H5 121(2) C6 C5 H5 121(2) O1 C6 C5 123.5(3) O1 C6 C1 116.7(3) C5 C6 C1 119.7(3) O1 C7 C8 109.5(2) O1 C7 H7A 104(2) C8 C7 H7A 111(2) O1 C7 H7B 108(2) C8 C7 H7B 114(2) H7A C7 H7B 109(3) N2 C8 C7 111.3(3) N2 C8 H8A 111(3) C7 C8 H8A 104(3) N2 C8 H8B 112(2) C7 C8 H8B 107(2) H8A C8 H8B 111(3) N2 C9 C10 111.0(3) N2 C9 H9A 107(2) C10 C9 H9A 108(2) N2 C9 H9B 111(2) C10 C9 H9B 108(2) H9A C9 H9B 112(3) N1 C10 C11 113.3(3) N1 C10 C9 105.7(3) C11 C10 C9 111.6(3) N1 C10 H10 112(2) C11 C10 H10 105.3(19) C9 C10 H10 109.6(18) C10 C11 C12 112.0(2) C10 C11 H11A 109(2) C12 C11 H11A 110(2) C10 C11 H11B 110(2) C12 C11 H11B 111(2) H11A C11 H11B 106(3) C14 C12 C13 109.4(3) C14 C12 C11 111.1(3) C13 C12 C11 111.6(3) C14 C12 H12 107.4(19) C13 C12 H12 107(2) C11 C12 H12 110.6(19) C12 C13 H13A 113(3) C12 C13 H13B 111(3) H13A C13 H13B 106(4) C12 C13 H13C 113(3) H13A C13 H13C 104(4) H13B C13 H13C 109(4) C12 C14 H14A 111(3) C12 C14 H14B 110(3) H14A C14 H14B 104(4) C12 C14 H14C 111(3) H14A C14 H14C 107(4) H14B C14 H14C 113(4) N2 C15 H15A 109.5 N2 C15 H15B 109.5 H15A C15 H15B 109.5 N2 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C4 1.906(3) S1 O2 1.433(2) S1 O3 1.434(2) S1 N1 1.625(3) S1 C1 1.776(3) O1 C6 1.363(4) O1 C7 1.450(4) N1 C10 1.490(4) N1 H1N 0.73(4) N2 C15 1.454(4) N2 C9 1.458(4) N2 C8 1.466(4) C1 C2 1.394(5) C1 C6 1.405(4) C2 C3 1.384(5) C2 H2 0.95(4) C3 C4 1.383(5) C3 H3 0.95(4) C4 C5 1.390(5) C5 C6 1.393(5) C5 H5 0.86(4) C7 C8 1.513(4) C7 H7A 1.03(4) C7 H7B 0.99(4) C8 H8A 0.95(5) C8 H8B 0.94(4) C9 C10 1.537(4) C9 H9A 0.90(4) C9 H9B 0.96(4) C10 C11 1.533(4) C10 H10 0.99(3) C11 C12 1.536(4) C11 H11A 0.95(4) C11 H11B 0.96(4) C12 C14 1.520(5) C12 C13 1.524(5) C12 H12 1.06(4) C13 H13A 0.92(4) C13 H13B 1.01(5) C13 H13C 0.94(5) C14 H14A 0.84(5) C14 H14B 0.91(5) C14 H14C 0.95(5) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 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 N1 H1N O1 0.73(4) 2.57(4) 2.942(4) 114(3) . N1 H1N N2 0.73(4) 2.34(4) 2.744(4) 117(3) . C2 H2 N1 0.95(4) 2.69(4) 3.554(4) 150(3) 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 O2 S1 N1 C10 -69.3(3) O3 S1 N1 C10 162.0(2) C1 S1 N1 C10 44.7(3) O2 S1 C1 C2 -13.4(3) O3 S1 C1 C2 115.6(3) N1 S1 C1 C2 -129.0(3) O2 S1 C1 C6 164.3(2) O3 S1 C1 C6 -66.7(3) N1 S1 C1 C6 48.7(3) C6 C1 C2 C3 -0.4(5) S1 C1 C2 C3 177.3(3) C1 C2 C3 C4 -2.3(5) C2 C3 C4 C5 2.1(5) C2 C3 C4 Br1 -177.3(2) C3 C4 C5 C6 0.8(5) Br1 C4 C5 C6 -179.8(2) C7 O1 C6 C5 35.4(4) C7 O1 C6 C1 -147.2(3) C4 C5 C6 O1 173.8(3) C4 C5 C6 C1 -3.5(4) C2 C1 C6 O1 -174.1(3) S1 C1 C6 O1 8.2(4) C2 C1 C6 C5 3.4(4) S1 C1 C6 C5 -174.3(2) C6 O1 C7 C8 75.7(3) C15 N2 C8 C7 98.0(3) C9 N2 C8 C7 -132.7(3) O1 C7 C8 N2 62.4(3) C15 N2 C9 C10 -159.5(3) C8 N2 C9 C10 71.3(3) S1 N1 C10 C11 82.8(3) S1 N1 C10 C9 -154.7(2) N2 C9 C10 N1 51.2(3) N2 C9 C10 C11 174.7(3) N1 C10 C11 C12 -157.7(3) C9 C10 C11 C12 83.2(3) C10 C11 C12 C14 -163.8(3) C10 C11 C12 C13 73.7(3)