#------------------------------------------------------------------------------ #$Date: 2019-11-23 18:51:17 +0200 (Sat, 23 Nov 2019) $ #$Revision: 234520 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/62/4036294.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_4036294 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 'C18 H27 Br N2 O3 S' _chemical_formula_weight 431.38 _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 difmap _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 9.6663(19) _cell_length_b 13.656(3) _cell_length_c 14.923(3) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.03 _cell_measurement_theta_min 4.39 _cell_volume 1969.9(7) _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 'Bruker SHELXTL' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.980 _diffrn_measurement_device_type 'Bruker Platinum 135 CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_unetI/netI 0.0290 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11456 _diffrn_reflns_point_group_measured_fraction_full 0.972 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 66.000 _diffrn_reflns_theta_max 68.020 _diffrn_reflns_theta_min 4.389 _diffrn_source 'Bruker MicroStar microfocus rotating anode' _exptl_absorpt_coefficient_mu 3.993 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.670 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.455 _exptl_crystal_description Needle _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.370 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.422 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 1377 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.029(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 334 _refine_ls_number_reflns 3417 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0213 _refine_ls_R_factor_gt 0.0210 _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^)+(0.0119P)^2^+1.0261P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.0518 _reflns_Friedel_coverage 0.695 _reflns_Friedel_fraction_full 0.943 _reflns_Friedel_fraction_max 0.914 _reflns_number_gt 3378 _reflns_number_total 3417 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo5b01429_si_002.cif _cod_data_source_block v40b_Cmpd_6p _cod_database_code 4036294 _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 0.320 _shelx_estimated_absorpt_t_max 0.857 _shelxl_version_number 2013-4 _shelx_res_file ; TITL C18H27BrN2O3S CELL 1.54178 9.66630 13.65570 14.92330 90.0000 90.0000 90.0000 ZERR 4.00 0.00190 0.00270 0.00290 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 72 108 8 12 4 4 TEMP -173.16C SIZE 0.04 0.055 0.37 ACTA 132. WPDB -2 L.S. 8 FMAP -2 PLAN 20 BOND $H CONF HTAB N1 O1 HTAB N1 N2 EQIV $1 x+1/2, -y+1/2, -z HTAB C5 O3_$1 EQIV $2 x-1/2, -y+1/2, -z HTAB C7 Br_$2 HTAB C7 O3_$1 EQIV $3 -x, y-1/2, -z+1/2 HTAB C13 O2_$3 EQIV $4 -x+1/2, -y+1, z+1/2 HTAB C16 Br_$4 HTAB C16 O2 HTAB WGHT 0.011900 1.026100 FVAR 0.19067 BR 6 0.421614 0.522563 -0.033500 11.00000 0.02746 0.02720 = 0.06028 0.01402 -0.00538 -0.00184 S 5 0.001296 0.284487 0.220272 11.00000 0.02235 0.03450 = 0.02307 0.00000 -0.00270 0.00859 O1 4 0.155772 0.206335 0.069249 11.00000 0.02222 0.02475 = 0.02483 -0.00104 0.00159 -0.00068 O2 4 -0.027091 0.347125 0.295311 11.00000 0.03593 0.03913 = 0.02675 -0.00401 -0.00287 0.01593 O3 4 -0.111284 0.251805 0.164981 11.00000 0.02066 0.05050 = 0.02913 0.00171 -0.00470 0.00517 N1 3 0.078109 0.186547 0.256712 11.00000 0.02112 0.02880 = 0.01977 -0.00122 0.00010 0.00478 H1N 2 0.093823 0.153873 0.211984 11.00000 0.02980 N2 3 0.305244 0.076891 0.202491 11.00000 0.01954 0.02390 = 0.02187 -0.00022 0.00425 -0.00179 C1 1 0.119446 0.349682 0.151395 11.00000 0.02549 0.02969 = 0.02567 0.00143 -0.00907 0.00561 C2 1 0.142791 0.448539 0.166180 11.00000 0.03417 0.02989 = 0.03257 -0.00117 -0.00994 0.01332 H2 2 0.100284 0.475765 0.210245 11.00000 0.02698 C3 1 0.232844 0.500776 0.111896 11.00000 0.03891 0.02246 = 0.04451 0.00300 -0.01577 0.00386 H3 2 0.239000 0.566313 0.121127 11.00000 0.03832 C4 1 0.299118 0.452599 0.042742 11.00000 0.02672 0.02620 = 0.03702 0.00736 -0.01181 0.00110 C5 1 0.277846 0.353848 0.025133 11.00000 0.02492 0.02851 = 0.02856 0.00461 -0.00393 0.00283 H5 2 0.321259 0.321385 -0.025743 11.00000 0.03368 C6 1 0.187336 0.302004 0.079825 11.00000 0.02191 0.02513 = 0.02585 0.00313 -0.00660 0.00249 C7 1 0.248606 0.143211 0.019459 11.00000 0.02459 0.02953 = 0.02017 -0.00267 0.00311 -0.00252 H7A 2 0.204287 0.076553 0.024754 11.00000 0.01624 H7B 2 0.252622 0.161981 -0.046178 11.00000 0.02064 C8 1 0.395356 0.139400 0.055495 11.00000 0.02259 0.02564 = 0.02474 0.00027 0.00542 -0.00311 H8A 2 0.442419 0.078748 0.027268 11.00000 0.02381 H8B 2 0.441427 0.195114 0.034868 11.00000 0.03234 C9 1 0.410500 0.138969 0.158335 11.00000 0.02156 0.02703 = 0.02397 -0.00073 0.00299 -0.00291 H9 2 0.395238 0.205913 0.178589 11.00000 0.02336 C10 1 0.559258 0.111186 0.184919 11.00000 0.02128 0.04848 = 0.02678 -0.00002 0.00161 -0.00490 H10A 2 0.571264 0.125148 0.251425 11.00000 0.03041 H10B 2 0.625753 0.155128 0.152159 11.00000 0.03158 C11 1 0.587341 0.002275 0.170109 11.00000 0.02282 0.05458 = 0.02873 0.00114 0.00195 0.01186 H11A 2 0.680377 -0.011098 0.191234 11.00000 0.03813 H11B 2 0.590303 -0.013511 0.106829 11.00000 0.03952 C12 1 0.479403 -0.059872 0.217533 11.00000 0.03640 0.03440 = 0.02902 0.00138 0.00473 0.01151 H12A 2 0.490124 -0.051565 0.281416 11.00000 0.02973 H12B 2 0.498895 -0.131372 0.204509 11.00000 0.02672 C13 1 0.334438 -0.028147 0.188914 11.00000 0.02709 0.02428 = 0.02706 -0.00007 0.00565 -0.00071 H13A 2 0.319730 -0.043962 0.120572 11.00000 0.02329 H13B 2 0.266655 -0.063095 0.223346 11.00000 0.03036 C14 1 0.286586 0.100285 0.297846 11.00000 0.02441 0.02611 = 0.02074 0.00229 0.00140 0.00379 H14A 2 0.228879 0.047846 0.322451 11.00000 0.02288 H14B 2 0.375429 0.106968 0.331033 11.00000 0.02956 C15 1 0.205300 0.195856 0.311778 11.00000 0.01796 0.02535 = 0.02207 0.00349 -0.00011 0.00102 H15 2 0.266827 0.252476 0.290578 11.00000 0.01845 C16 1 0.171485 0.213934 0.411229 11.00000 0.02299 0.02407 = 0.02228 0.00005 -0.00246 0.00697 H16 2 0.111196 0.262607 0.410292 11.00000 0.01884 C17 1 0.102330 0.127225 0.456109 11.00000 0.03738 0.03292 = 0.02405 0.00223 0.00604 0.00085 H17A 2 0.071452 0.145138 0.515023 11.00000 0.02684 H17B 2 0.168667 0.072748 0.462607 11.00000 0.03990 H17C 2 0.015327 0.102146 0.420168 11.00000 0.05410 C18 1 0.299577 0.247092 0.462335 11.00000 0.03270 0.03860 = 0.03276 -0.00802 -0.00768 0.00195 H18A 2 0.369427 0.195465 0.464542 11.00000 0.04260 H18B 2 0.272110 0.261057 0.529628 11.00000 0.03616 H18C 2 0.343676 0.305393 0.433730 11.00000 0.04246 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM C18H27BrN2O3S REM R1 = 0.0210 for 3378 Fo > 4sig(Fo) and 0.0213 for all 3417 data REM 334 parameters refined using 0 restraints END WGHT 0.0116 1.0356 REM Instructions for potential hydrogen bonds HTAB N1 O1 HTAB N1 N2 HTAB C5 O3_$1 HTAB C7 Br_$2 HTAB C7 O3_$1 HTAB C13 O2_$3 HTAB C16 Br_$4 HTAB C16 O2 REM Highest difference peak 0.422, deepest hole -0.554, 1-sigma level 0.045 Q1 1 0.4205 0.5039 -0.0825 11.00000 0.05 -0.55 Q2 1 0.4148 0.5403 0.0226 11.00000 0.05 0.42 Q3 1 0.4752 0.4789 -0.0240 11.00000 0.05 -0.36 Q4 1 0.4703 0.5609 -0.0295 11.00000 0.05 -0.33 Q5 1 0.4156 0.4310 -0.0214 11.00000 0.05 -0.26 Q6 1 -0.0404 0.2450 0.2356 11.00000 0.05 -0.23 Q7 1 0.0826 0.2017 0.3818 11.00000 0.05 -0.21 Q8 1 0.1927 0.3830 0.1148 11.00000 0.05 -0.21 Q9 1 0.3644 0.4932 -0.0027 11.00000 0.05 -0.21 Q10 1 0.5031 0.6043 -0.0192 11.00000 0.05 0.20 Q11 1 0.5077 0.4363 -0.0378 11.00000 0.05 0.20 Q12 1 0.2992 0.4034 0.0381 11.00000 0.05 0.19 Q13 1 0.3300 0.5995 -0.0355 11.00000 0.05 0.19 Q14 1 0.4103 0.4813 -0.0376 11.00000 0.05 0.19 Q15 1 0.3555 0.5585 -0.0126 11.00000 0.05 -0.19 Q16 1 0.0495 0.3027 0.2572 11.00000 0.05 -0.19 Q17 1 0.5681 0.4808 -0.0403 11.00000 0.05 0.19 Q18 1 0.0241 0.2610 0.1796 11.00000 0.05 -0.19 Q19 1 0.3282 0.4380 -0.0408 11.00000 0.05 0.17 Q20 1 0.0794 0.4316 0.3058 11.00000 0.05 0.17 ; _shelx_res_checksum 52815 _shelx_hkl_file ; 1 0 0 0.02 0.03 -1 0 0 -0.02 0.03 2 0 0 38.15 1.57 -2 0 0 37.50 1.65 -3 0 0 0.16 0.07 3 0 0 0.00 0.06 4 0 0 23.04 1.09 -4 0 0 23.44 1.10 4 0 0 23.42 1.07 4 0 0 21.58 0.97 -5 0 0 -0.12 0.07 5 0 0 -0.08 0.07 5 0 0 -0.08 0.08 7 0 0 0.12 0.11 8 0 0 21.68 1.17 9 0 0 0.05 0.12 9 0 0 0.03 0.11 9 0 0 0.05 0.14 9 0 0 0.34 0.17 10 0 0 92.72 3.89 10 0 0 92.74 3.87 10 0 0 87.85 3.60 10 0 0 95.83 4.74 11 0 0 0.06 0.10 11 0 0 0.03 0.10 11 0 0 -0.01 0.10 11 0 0 0.05 0.08 0 1 0 0.08 0.02 0 -1 0 0.09 0.02 0 -1 0 0.06 0.02 1 -1 0 34.85 1.41 -1 1 0 33.92 1.45 -1 -1 0 34.23 1.48 -2 -1 0 88.52 3.75 2 -1 0 88.03 3.57 -2 1 0 87.79 3.73 3 -1 0 354.44 14.07 -3 -1 0 349.66 14.81 -3 1 0 353.06 14.78 4 1 0 0.22 0.11 4 1 0 0.23 0.09 4 -1 0 0.24 0.10 4 -1 0 0.21 0.11 4 -1 0 0.09 0.08 4 1 0 0.11 0.09 -4 -1 0 0.17 0.11 5 -1 0 91.77 3.85 5 1 0 90.46 3.84 5 1 0 91.27 4.04 5 -1 0 94.21 4.02 -5 -1 0 91.48 4.04 6 1 0 1.38 0.21 6 -1 0 1.48 0.20 7 -1 0 40.31 1.94 7 1 0 41.47 1.98 8 1 0 11.19 0.73 8 -1 0 11.42 0.71 9 1 0 65.88 2.87 9 1 0 62.65 3.38 9 -1 0 66.18 2.79 9 -1 0 64.71 2.59 9 -1 0 64.44 3.36 9 1 0 63.79 2.60 9 1 0 63.08 2.80 9 -1 0 63.65 2.82 10 -1 0 18.86 0.97 10 -1 0 19.92 1.14 10 1 0 19.75 1.17 10 1 0 18.97 0.90 10 1 0 20.14 1.00 10 -1 0 18.86 0.89 10 -1 0 19.85 1.00 11 -1 0 28.52 1.21 11 1 0 28.59 1.21 11 -1 0 29.42 1.32 11 -1 0 30.31 1.58 11 1 0 28.44 1.59 11 1 0 30.23 1.33 11 -1 0 28.37 1.30 0 -2 0 26.40 1.16 0 -2 0 27.05 1.11 1 -2 0 351.33 13.89 -1 -2 0 348.81 14.63 -2 2 0 14.23 0.65 2 -2 0 14.65 0.67 -2 -2 0 14.58 0.70 3 -2 0 32.54 1.40 -3 2 0 31.84 1.42 -3 -2 0 32.14 1.47 4 2 0 38.71 1.60 4 -2 0 40.18 1.71 -4 -2 0 40.81 1.80 4 2 0 37.90 1.77 4 -2 0 38.50 1.74 4 -2 0 36.07 1.56 4 2 0 38.89 1.69 -5 -2 0 25.97 1.28 5 2 0 24.92 1.24 5 -2 0 25.05 1.22 5 -2 0 25.40 1.21 6 2 0 325.31 14.20 6 -2 0 339.06 14.17 7 2 0 1.66 0.28 7 2 0 1.89 0.26 7 -2 0 1.78 0.23 8 -2 0 114.27 5.06 8 2 0 113.87 5.10 8 2 0 113.46 4.96 9 2 0 3.44 0.36 9 -2 0 3.70 0.34 9 2 0 3.60 0.38 9 -2 0 3.64 0.36 9 -2 0 3.35 0.33 9 -2 0 3.20 0.28 9 2 0 3.43 0.32 10 -2 0 6.39 0.46 10 2 0 6.59 0.47 10 2 0 6.53 0.52 10 -2 0 6.04 0.39 10 2 0 6.14 0.41 10 -2 0 6.46 0.44 10 -2 0 6.54 0.45 11 -2 0 6.16 0.40 11 2 0 6.17 0.46 11 -2 0 6.43 0.43 11 2 0 6.27 0.36 11 -2 0 5.80 0.38 11 -2 0 6.14 0.35 11 2 0 6.67 0.41 0 -3 0 -0.07 0.06 1 -3 0 747.13 29.31 -1 -3 0 727.73 30.93 -2 -3 0 69.18 3.02 2 -3 0 71.06 2.88 3 -3 0 673.81 26.05 -3 -3 0 660.58 27.41 3 3 0 630.95 24.79 4 -3 0 266.41 10.63 4 3 0 258.13 10.10 -4 -3 0 270.30 11.19 4 -3 0 261.53 11.23 5 3 0 185.61 8.02 5 -3 0 185.31 7.58 5 -3 0 186.59 7.97 6 3 0 22.30 1.19 6 -3 0 23.59 1.15 7 -3 0 50.61 2.27 7 3 0 46.03 2.27 7 3 0 48.42 2.33 8 -3 0 3.31 0.62 8 3 0 3.03 0.38 8 -3 0 2.99 0.33 8 3 0 2.82 0.44 8 3 0 2.92 0.38 9 3 0 80.93 3.79 9 -3 0 86.99 3.63 9 -3 0 84.53 3.58 9 -3 0 89.66 4.33 9 3 0 85.10 3.65 9 3 0 82.22 3.59 9 -3 0 82.67 3.33 10 -3 0 1.17 0.21 10 -3 0 1.08 0.17 10 3 0 1.12 0.27 10 -3 0 0.93 0.21 10 -3 0 1.03 0.18 10 3 0 1.08 0.20 10 3 0 1.19 0.23 11 -3 0 24.03 1.27 11 -3 0 22.09 1.00 11 -3 0 24.23 1.09 11 -3 0 25.07 1.29 11 3 0 23.10 1.01 11 3 0 24.84 1.12 11 -3 0 22.47 1.08 0 -4 0 404.28 16.86 1 -4 0 4.73 0.26 -1 -4 0 4.50 0.27 2 -4 0 29.89 1.25 -2 4 0 26.54 1.17 2 4 0 29.06 1.21 -2 -4 0 29.06 1.31 -3 -4 0 208.55 8.92 3 -4 0 213.78 8.47 3 -4 0 212.69 8.96 3 4 0 211.12 8.08 -3 4 0 204.67 8.02 -4 -4 0 28.90 1.41 4 -4 0 29.01 1.34 4 4 0 28.28 1.27 4 -4 0 29.27 1.33 5 4 0 131.77 5.66 5 -4 0 125.67 5.57 6 4 0 4.24 0.39 6 -4 0 4.04 0.33 7 4 0 129.54 5.66 7 4 0 135.05 5.88 7 -4 0 130.37 5.77 8 4 0 22.31 1.27 8 -4 0 22.19 1.09 8 -4 0 22.80 1.22 8 -4 0 21.02 1.17 8 -4 0 22.18 1.85 8 4 0 22.03 1.25 8 -4 0 21.70 1.01 8 4 0 22.21 1.18 8 4 0 21.16 1.23 9 -4 0 27.93 1.51 9 -4 0 26.97 1.21 9 4 0 27.51 1.39 9 -4 0 27.64 1.34 9 4 0 27.10 1.44 9 -4 0 29.63 2.16 9 4 0 27.14 1.48 9 -4 0 27.56 1.31 10 -4 0 9.57 0.56 10 4 0 9.41 0.55 10 4 0 9.16 0.69 10 4 0 9.59 0.61 10 -4 0 10.02 0.58 10 -4 0 10.01 0.52 10 4 0 9.59 0.68 10 -4 0 10.26 0.61 11 -4 0 0.85 0.14 11 -4 0 0.87 0.13 11 4 0 0.68 0.14 11 -4 0 0.87 0.16 11 -4 0 0.85 0.14 11 4 0 0.83 0.18 0 5 0 0.22 0.09 1 5 0 102.16 3.98 1 -5 0 101.02 4.10 -1 -5 0 104.99 4.32 -1 5 0 98.28 3.96 2 -5 0 76.75 3.47 2 -5 0 82.97 3.28 -2 5 0 78.11 3.13 2 5 0 80.13 3.16 -2 -5 0 80.00 3.45 3 -5 0 71.87 3.10 -3 -5 0 70.07 3.12 3 5 0 71.19 2.85 -3 -5 0 66.47 2.90 -3 5 0 70.46 2.80 3 -5 0 73.85 2.96 -4 -5 0 104.70 4.72 4 -5 0 106.76 4.47 4 -5 0 108.81 4.68 4 5 0 110.73 4.29 5 5 0 110.06 4.42 5 -5 0 110.37 4.81 6 5 0 2.67 0.34 6 -5 0 3.18 0.30 6 5 0 3.15 0.36 7 5 0 30.67 1.58 7 5 0 26.71 1.48 7 5 0 28.46 1.51 7 -5 0 29.23 1.45 8 5 0 0.58 0.22 8 -5 0 0.47 0.18 8 -5 0 0.55 0.14 8 -5 0 0.59 0.15 8 5 0 0.32 0.19 8 5 0 0.39 0.23 8 -5 0 0.41 0.18 8 -5 0 0.54 0.18 8 5 0 0.32 0.20 8 -5 0 0.44 0.33 9 -5 0 45.89 2.07 9 5 0 45.56 2.16 9 -5 0 47.08 2.07 9 5 0 45.18 2.25 9 -5 0 45.44 3.26 9 -5 0 47.34 2.42 9 5 0 48.20 2.17 9 -5 0 47.11 1.92 10 -5 0 16.01 0.76 10 5 0 15.48 0.97 10 5 0 16.60 0.89 10 -5 0 16.67 0.82 10 -5 0 17.05 0.93 10 5 0 16.36 0.80 10 -5 0 14.71 1.29 10 5 0 16.40 0.94 10 -5 0 16.33 0.83 11 5 0 0.08 0.11 11 -5 0 0.09 0.08 0 -6 0 235.34 9.60 0 6 0 251.94 9.36 1 6 0 52.97 2.05 -1 -6 0 46.90 2.07 -1 6 0 49.66 2.04 1 -6 0 49.54 2.06 1 -6 0 48.05 2.23 2 -6 0 54.72 2.54 -2 6 0 58.00 2.31 2 6 0 57.67 2.33 2 -6 0 56.67 2.36 -2 -6 0 54.99 2.37 3 -6 0 123.37 5.30 -3 -6 0 117.77 4.92 3 -6 0 124.06 4.99 3 6 0 125.95 4.83 -3 6 0 123.83 4.79 -3 -6 0 115.94 5.26 4 -6 0 28.58 1.35 -4 -6 0 26.85 1.29 4 6 0 28.33 1.32 5 -6 0 29.41 1.44 5 6 0 29.89 1.42 6 6 0 180.08 7.62 6 -6 0 171.79 7.47 6 6 0 164.31 7.28 7 6 0 7.38 0.66 7 6 0 7.30 0.61 7 6 0 7.48 0.64 7 -6 0 6.89 0.53 8 6 0 14.50 0.95 8 -6 0 14.94 0.82 8 -6 0 15.24 0.82 8 6 0 14.86 0.95 8 -6 0 12.57 1.37 8 -6 0 14.78 0.75 8 6 0 15.54 0.93 8 -6 0 15.88 0.86 9 -6 0 8.54 1.00 9 6 0 9.23 0.71 9 -6 0 9.72 0.57 9 6 0 9.47 0.71 9 -6 0 9.41 0.53 9 6 0 9.97 0.68 9 -6 0 9.86 0.61 9 -6 0 9.49 0.59 10 -6 0 1.26 0.19 10 -6 0 0.99 0.32 10 6 0 1.18 0.21 10 -6 0 1.24 0.22 10 -6 0 1.40 0.18 10 6 0 1.17 0.23 10 -6 0 1.34 0.14 10 6 0 1.18 0.27 0 -7 0 0.12 0.09 0 7 0 0.01 0.08 -1 7 0 132.88 5.18 1 7 0 132.44 5.18 -1 -7 0 133.89 5.31 1 -7 0 127.20 5.27 2 7 0 441.85 16.28 2 -7 0 412.10 16.98 2 -7 0 410.79 18.12 -2 7 0 433.81 16.27 -2 -7 0 430.90 16.73 -3 7 0 20.87 1.02 -3 -7 0 20.85 1.04 3 -7 0 21.14 1.10 3 7 0 21.48 1.05 4 -7 0 29.77 1.47 4 7 0 30.13 1.43 -4 -7 0 28.76 1.39 5 7 0 8.26 0.62 5 -7 0 8.32 0.58 5 7 0 8.59 0.62 6 7 0 1.36 0.32 6 7 0 1.80 0.40 6 -7 0 1.36 0.27 6 7 0 1.53 0.31 7 -7 0 0.80 0.19 7 7 0 0.71 0.28 7 7 0 0.63 0.26 7 -7 0 1.10 0.47 7 7 0 1.15 0.30 7 7 0 0.55 0.22 7 -7 0 1.11 0.24 7 -7 0 0.47 0.21 8 -7 0 38.55 1.72 8 -7 0 37.44 1.75 8 7 0 39.53 1.92 8 -7 0 37.98 2.00 8 -7 0 34.90 2.79 8 7 0 38.24 1.86 8 -7 0 39.38 1.63 8 7 0 36.60 1.86 9 7 0 17.39 1.07 9 -7 0 20.24 1.01 9 7 0 21.03 1.12 9 7 0 20.54 1.15 9 -7 0 20.13 1.08 9 -7 0 20.06 0.93 9 -7 0 18.92 1.63 9 -7 0 20.98 0.97 10 -7 0 16.52 1.33 10 7 0 18.75 0.94 10 -7 0 17.89 0.81 10 -7 0 18.15 0.79 10 7 0 15.36 0.79 10 -7 0 17.43 0.85 0 8 0 49.78 2.14 0 -8 0 50.84 2.17 -1 -8 0 86.53 3.54 -1 8 0 86.50 3.47 1 8 0 85.25 3.46 1 -8 0 81.42 3.50 2 8 0 20.87 1.05 -2 8 0 21.26 1.05 -2 -8 0 21.30 1.06 3 -8 0 9.77 0.65 3 8 0 9.79 0.64 -3 -8 0 9.83 0.62 -3 8 0 9.97 0.63 4 8 0 15.05 0.90 -4 -8 0 14.97 0.85 4 -8 0 15.34 0.91 5 -8 0 278.91 11.61 -5 -8 0 261.65 10.11 5 8 0 263.88 10.53 6 8 0 144.08 6.13 6 -8 0 153.18 9.02 6 8 0 140.42 5.81 6 -8 0 138.15 6.31 6 8 0 135.68 6.43 7 -8 0 45.79 1.91 7 8 0 48.89 2.24 7 8 0 40.09 2.17 7 8 0 47.98 2.18 7 -8 0 44.91 2.06 7 -8 0 43.99 2.36 7 -8 0 46.13 3.30 8 8 0 0.51 0.24 8 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29.21 1.50 -5 -11 0 2.28 0.29 5 -11 0 2.57 0.26 5 11 0 2.56 0.38 6 -11 0 19.96 1.10 6 11 0 20.73 1.13 -6 -11 0 18.61 0.96 7 -11 0 2.07 0.20 7 11 0 2.01 0.31 8 -11 0 8.42 0.78 0 -12 0 46.10 1.91 0 -12 0 45.82 1.95 0 -12 0 45.61 1.95 0 -12 0 45.58 2.13 -1 -12 0 15.23 0.82 1 -12 0 15.82 0.84 -1 -12 0 14.49 0.91 -1 -12 0 14.88 0.75 1 -12 0 14.68 0.73 -1 -12 0 15.14 0.82 2 -12 0 11.33 0.70 -2 -12 0 11.86 0.79 2 -12 0 10.92 0.80 -2 -12 0 11.78 0.62 -2 -12 0 11.56 0.69 2 -12 0 11.35 0.58 3 -12 0 0.26 0.16 -3 -12 0 0.17 0.14 -3 -12 0 0.18 0.11 3 -12 0 0.45 0.18 3 -12 0 0.26 0.14 4 -12 0 0.23 0.17 4 -12 0 0.41 0.16 4 12 0 0.45 0.19 -4 -12 0 0.20 0.14 5 12 0 18.25 1.02 5 -12 0 17.43 1.04 -5 -12 0 18.02 0.91 6 12 0 18.30 0.98 -6 -12 0 17.41 0.87 6 -12 0 18.27 1.02 7 12 0 64.58 2.74 7 -12 0 62.55 3.22 0 -13 0 0.17 0.13 0 -13 0 0.06 0.16 0 -13 0 0.07 0.09 0 -13 0 0.02 0.11 -1 -13 0 0.48 0.16 -1 -13 0 0.43 0.16 1 -13 0 0.40 0.12 -1 -13 0 0.48 0.18 1 -13 0 0.35 0.18 -1 -13 0 0.48 0.14 1 -13 0 0.48 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0.10 0.09 -5 0 -1 0.11 0.09 5 0 1 0.14 0.09 6 0 -1 3.82 0.32 6 0 1 3.71 0.32 7 0 -1 45.04 2.13 7 0 1 44.93 2.13 8 0 1 124.57 5.49 8 0 -1 123.23 5.48 9 0 -1 17.48 0.93 9 0 -1 17.37 1.07 9 0 1 17.74 0.94 9 0 1 17.52 1.07 9 0 1 17.37 0.94 9 0 -1 17.72 0.97 9 0 1 17.66 0.86 10 0 -1 48.24 2.13 10 0 1 48.85 2.14 10 0 1 48.92 1.99 10 0 -1 50.01 2.18 10 0 1 49.55 2.59 10 0 -1 47.85 2.59 10 0 1 46.70 2.12 11 0 -1 5.09 0.35 11 0 -1 5.08 0.40 11 0 -1 5.02 0.36 11 0 1 5.38 0.32 11 0 1 5.31 0.36 11 0 1 5.15 0.39 0 -1 1 119.70 4.96 0 -1 -1 116.94 4.71 -1 1 1 420.23 16.92 -1 -1 -1 430.82 16.98 1 -1 1 421.90 16.08 -1 -1 1 366.40 16.92 1 -1 -1 375.11 16.01 2 -1 1 103.66 4.13 -2 1 1 102.08 4.32 -2 -1 -1 105.56 4.36 2 1 1 101.39 4.11 -2 1 -1 101.35 4.33 2 -1 -1 101.30 4.14 -2 -1 1 102.37 4.35 3 -1 1 23.71 1.07 -3 -1 -1 24.26 1.15 -3 1 1 23.03 1.10 -3 1 -1 25.07 1.13 -3 -1 1 24.50 1.13 3 -1 -1 24.68 1.10 3 1 1 23.93 1.06 4 1 -1 34.98 1.61 -4 1 1 35.85 1.60 4 -1 1 33.74 1.60 4 1 -1 32.19 1.45 4 1 -1 35.27 1.57 4 -1 1 35.26 1.55 -4 -1 -1 35.96 1.64 4 -1 -1 34.12 1.44 -4 1 -1 37.20 1.63 4 -1 -1 34.81 1.60 -4 -1 1 37.59 1.64 4 1 1 34.71 1.61 4 -1 -1 36.35 1.58 4 1 1 35.32 1.53 5 -1 1 55.03 2.26 5 -1 1 54.69 2.35 5 1 -1 54.16 2.13 5 1 -1 53.38 2.29 -5 -1 -1 56.34 2.41 5 1 -1 55.09 2.36 5 -1 -1 48.55 2.33 5 -1 -1 47.32 2.10 -5 -1 1 48.83 2.36 5 -1 -1 48.66 2.28 5 1 1 48.83 2.35 -5 1 -1 52.07 2.41 6 1 -1 0.59 0.16 6 -1 1 0.48 0.15 6 -1 -1 0.59 0.15 6 1 1 0.69 0.16 7 1 -1 130.62 5.58 7 -1 1 128.20 5.55 7 -1 -1 124.46 5.54 7 1 1 116.05 5.39 7 1 1 131.64 5.58 8 1 -1 15.47 0.91 8 -1 1 15.50 0.88 8 1 1 15.31 0.91 8 -1 -1 14.75 0.87 9 -1 1 24.66 1.33 9 1 -1 23.09 1.15 9 -1 1 23.55 1.06 9 -1 1 25.09 1.16 9 -1 1 24.09 1.17 9 1 -1 23.69 1.36 9 1 -1 24.58 1.20 9 1 1 21.69 1.15 9 -1 -1 21.85 1.32 9 1 1 22.39 1.35 9 -1 -1 21.43 1.13 9 -1 -1 21.83 1.17 9 1 1 20.95 1.05 10 -1 1 0.24 0.13 10 -1 1 0.19 0.13 10 1 -1 0.16 0.14 10 1 -1 0.10 0.14 10 -1 1 0.10 0.12 10 1 -1 0.15 0.14 10 -1 1 0.07 0.09 10 -1 -1 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3.46 5 7 -4 18.25 1.16 -5 -7 -4 18.49 1.04 5 -7 4 19.95 1.09 -5 7 4 19.61 0.99 -5 -7 -4 19.21 0.98 5 7 -4 19.78 1.08 5 7 4 18.29 1.07 5 7 4 19.28 1.08 6 -7 4 45.54 2.17 -6 7 4 44.19 2.01 6 7 -4 44.48 2.24 6 -7 4 49.35 3.13 6 7 -4 45.61 2.26 6 7 -4 43.57 2.08 -6 -7 -4 43.02 1.91 6 7 4 40.97 2.11 6 7 4 39.82 2.15 6 -7 -4 46.88 3.26 6 7 4 40.72 2.12 7 -7 4 19.08 0.98 7 7 -4 20.12 1.26 -7 -7 -4 18.50 1.00 7 -7 4 19.37 0.94 7 -7 4 18.68 1.61 7 -7 4 19.71 1.03 7 7 -4 19.82 1.15 7 -7 -4 19.73 1.21 7 7 4 22.14 1.18 7 7 4 20.17 1.09 7 -7 -4 20.23 1.83 7 7 4 20.99 1.22 8 7 -4 47.05 2.18 8 -7 4 48.45 1.98 8 -7 4 48.44 2.08 8 -7 4 47.04 2.13 8 7 -4 45.41 2.39 8 -7 4 48.88 3.24 8 -7 -4 46.76 2.55 8 7 4 46.40 2.26 8 7 4 47.75 2.24 8 7 4 49.35 2.18 9 7 -4 25.37 1.28 9 -7 4 24.73 1.23 9 -7 4 25.21 1.14 9 -7 4 26.20 1.86 9 -7 4 25.88 1.18 9 7 4 27.06 1.25 9 7 4 26.49 1.35 9 7 4 25.97 1.34 9 -7 -4 26.93 1.44 10 -7 4 10.07 0.51 10 -7 4 9.81 0.55 10 -7 4 10.46 0.52 10 7 4 10.56 0.55 10 -7 -4 11.26 0.61 10 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44.21 2.13 7 8 4 43.01 2.13 7 8 4 41.65 2.05 7 -8 -4 41.66 2.39 8 -8 4 13.41 1.24 8 -8 4 16.18 0.78 8 -8 4 16.97 0.79 8 -8 4 15.84 0.85 8 8 -4 16.96 0.95 8 8 4 16.18 0.97 8 8 4 14.62 0.85 8 8 4 16.39 0.94 8 -8 -4 13.98 1.46 8 -8 -4 15.24 0.94 9 -8 4 28.90 1.35 9 -8 4 29.91 2.02 9 -8 4 27.87 1.25 9 8 -4 27.90 1.36 9 -8 4 29.58 1.29 9 8 4 29.50 1.42 9 -8 -4 30.85 1.57 9 8 4 30.32 1.36 0 9 -4 41.19 1.87 0 -9 -4 43.51 1.93 0 9 4 41.71 1.91 0 -9 4 42.60 1.92 -1 9 4 97.39 4.05 1 -9 4 97.40 4.11 -1 -9 -4 100.89 4.15 1 9 -4 98.61 4.02 -1 -9 4 102.78 4.14 1 9 4 95.25 4.02 -2 9 4 56.84 2.48 -2 -9 -4 56.02 2.52 2 9 -4 56.45 2.46 2 9 4 56.67 2.46 -2 -9 4 56.73 2.50 -3 9 4 83.52 3.46 -3 -9 -4 87.11 3.55 -3 -9 -4 82.55 3.30 3 9 -4 80.85 3.44 3 -9 4 81.09 3.29 -3 -9 4 76.03 3.24 -3 -9 4 82.02 3.50 -4 -9 -4 57.73 2.46 4 9 -4 54.91 2.42 -4 -9 -4 54.18 2.27 -4 9 4 56.56 2.41 4 -9 4 55.92 2.59 4 9 4 47.85 2.46 -4 -9 4 51.26 2.39 -4 -9 4 47.22 2.18 4 -9 -4 55.62 3.67 5 9 -4 32.57 1.67 5 -9 4 32.95 1.45 5 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29.07 1.38 2 10 -4 31.19 1.56 2 -10 4 30.54 1.45 -2 -10 -4 31.34 1.59 -2 10 4 32.59 1.59 2 10 4 34.72 1.60 -2 -10 4 36.30 1.42 2 -10 -4 33.80 1.37 -2 -10 4 35.35 1.46 3 10 -4 9.97 0.69 -3 -10 -4 9.60 0.61 3 -10 4 10.30 0.63 3 -10 4 9.69 0.52 -3 10 4 10.72 0.72 -3 -10 -4 10.52 0.71 -3 -10 4 8.80 0.57 -3 -10 4 9.01 0.54 -3 -10 4 9.20 0.66 3 -10 -4 8.35 0.49 -4 -10 -4 62.39 2.64 4 10 -4 60.45 2.67 4 -10 4 58.23 2.02 4 -10 4 58.65 3.00 4 -10 4 61.42 2.39 -4 -10 -4 57.52 2.41 -4 -10 4 50.19 2.54 4 -10 -4 58.53 3.91 -4 -10 4 49.64 2.33 5 -10 4 6.16 0.45 -5 -10 -4 5.94 0.47 5 10 -4 6.51 0.57 5 -10 -4 6.02 0.47 5 -10 -4 6.17 0.85 6 -10 4 0.93 0.17 -6 -10 -4 0.75 0.20 6 10 -4 1.12 0.29 6 -10 -4 0.83 0.17 6 10 4 0.90 0.28 6 -10 -4 0.49 0.37 6 10 4 1.07 0.24 -7 -10 -4 10.86 0.65 7 10 -4 10.63 0.71 7 10 4 11.97 0.69 7 -10 -4 12.33 0.71 7 10 4 12.19 0.78 8 -10 4 6.53 0.63 8 -10 -4 7.06 0.44 8 10 4 6.96 0.51 8 10 4 6.35 0.43 0 -11 4 0.16 0.13 0 -11 -4 0.14 0.09 0 -11 4 0.16 0.15 0 -11 4 0.15 0.09 0 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1.12 2 4 8 23.48 1.23 3 4 -8 90.69 3.61 3 -4 8 89.71 3.72 3 4 8 84.82 3.83 4 4 -8 27.15 1.33 4 4 8 27.60 1.49 4 4 8 27.11 1.41 5 4 -8 46.37 2.09 5 4 8 46.98 2.24 5 -4 -8 45.54 1.99 6 -4 8 2.34 0.24 6 -4 8 2.67 0.43 6 4 -8 1.57 0.38 6 4 -8 2.26 0.40 6 -4 -8 2.21 0.28 6 4 8 2.12 0.36 7 4 -8 40.57 1.87 7 -4 8 37.77 2.15 7 -4 8 38.39 1.73 7 -4 -8 38.12 1.72 7 4 8 40.60 2.01 7 4 8 40.02 1.99 8 -4 8 20.73 1.03 8 4 -8 21.92 1.16 8 -4 8 22.81 1.22 8 -4 -8 22.52 1.05 8 4 8 23.67 1.29 8 4 8 22.16 1.30 9 4 -8 27.29 1.23 9 4 -8 23.04 1.27 9 -4 8 25.59 1.14 9 4 8 24.78 1.47 9 4 8 29.34 1.44 9 -4 -8 27.17 1.13 9 -4 -8 22.98 1.23 0 -5 8 303.47 12.10 0 5 8 307.04 12.23 1 -5 8 67.09 2.83 1 5 8 65.50 2.95 -1 -5 8 64.86 2.81 2 -5 8 76.75 3.23 -2 5 8 77.95 3.08 -2 -5 8 73.85 3.21 2 5 8 75.27 3.38 3 5 -8 77.48 3.28 3 -5 8 76.04 3.36 -3 5 8 84.41 3.25 3 5 8 79.52 3.55 4 5 -8 4.65 0.43 4 5 8 3.84 0.41 5 5 -8 6.27 0.53 5 -5 -8 5.92 0.42 5 5 8 5.61 0.52 5 -5 -8 6.57 0.93 6 5 -8 5.16 0.53 6 -5 8 4.91 0.36 6 -5 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42.85 2.36 7 -3 -9 39.83 1.81 7 3 9 42.11 2.11 8 3 -9 53.11 2.16 8 -3 9 45.98 2.58 8 -3 9 46.64 2.06 8 -3 -9 49.27 2.06 8 3 9 46.90 2.65 8 3 9 52.69 2.40 8 -3 -9 46.59 2.17 9 3 9 1.03 0.22 9 -3 -9 1.02 0.21 9 -3 -9 1.35 0.18 0 -4 9 72.64 3.08 0 4 9 71.97 3.16 1 -4 9 47.85 2.26 1 4 9 51.99 2.37 -1 -4 9 53.73 2.27 2 -4 9 22.33 1.09 -2 -4 9 19.57 1.05 2 4 9 19.42 1.15 3 -4 9 16.26 0.92 3 4 9 14.99 0.93 3 4 9 17.09 1.04 4 4 -9 2.17 0.31 4 4 9 1.64 0.30 4 4 9 1.81 0.39 5 -4 -9 42.15 1.85 5 4 9 42.84 2.10 6 4 -9 31.04 1.50 6 -4 9 28.06 1.35 6 4 9 31.14 1.62 6 -4 -9 29.60 1.37 7 4 -9 18.90 1.02 7 -4 9 17.64 0.87 7 -4 9 16.45 1.10 7 -4 -9 17.95 0.90 7 4 9 18.24 1.15 7 4 9 18.96 1.12 8 4 -9 13.69 0.78 8 -4 9 14.13 0.79 8 4 9 13.24 0.87 8 4 9 12.31 0.89 8 -4 -9 13.10 0.69 9 4 -9 0.59 0.16 9 4 -9 0.36 0.17 9 4 9 0.61 0.17 9 -4 -9 0.78 0.13 0 -5 9 6.20 0.48 0 5 9 6.09 0.56 1 -5 9 80.76 3.32 -1 -5 9 76.11 3.29 1 5 9 75.11 3.44 2 -5 9 77.59 3.41 2 5 9 82.68 3.60 -2 -5 9 79.72 3.40 3 -5 9 29.42 1.49 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7 -6 -9 4.95 0.34 -8 -6 -9 4.33 0.34 8 6 9 3.45 0.43 8 -6 -9 3.58 0.26 0 -7 9 0.10 0.11 0 -7 9 0.01 0.14 1 -7 9 69.52 3.00 1 -7 9 66.79 2.34 1 7 9 69.03 2.49 -1 -7 9 67.39 2.75 -1 -7 9 72.08 3.00 1 -7 -9 65.74 2.75 2 -7 9 17.11 0.76 2 -7 9 17.61 0.99 2 -7 -9 17.74 1.44 2 7 9 16.90 0.86 -2 -7 9 17.21 0.98 -2 -7 9 17.29 0.84 2 -7 -9 17.20 0.83 3 -7 9 59.65 2.10 -3 -7 9 61.17 2.48 3 7 9 57.58 2.21 3 -7 -9 61.53 2.45 3 -7 -9 61.33 4.00 -3 -7 9 58.83 2.66 4 -7 9 29.23 1.16 4 -7 9 29.21 1.37 -4 -7 9 29.98 1.34 4 -7 -9 31.83 2.29 4 7 9 27.37 1.50 4 -7 -9 29.79 1.30 -5 -7 -9 29.77 1.36 5 7 -9 28.89 1.54 5 -7 9 27.50 1.30 5 -7 -9 27.27 2.21 5 -7 -9 25.86 1.22 -6 -7 -9 8.61 0.58 6 -7 9 7.62 0.58 6 -7 -9 7.60 0.99 6 7 9 7.94 0.61 6 7 9 8.03 0.69 6 -7 -9 7.96 0.46 -7 -7 -9 25.51 1.18 7 7 9 24.78 1.30 7 7 9 25.75 1.35 7 -7 -9 21.84 1.96 7 -7 -9 25.73 1.08 8 -7 -9 5.22 0.30 8 7 9 5.27 0.48 0 -8 9 8.56 0.50 0 -8 -9 8.70 0.88 0 -8 9 9.13 0.56 0 -8 9 9.47 0.65 0 -8 9 9.43 0.50 0 -8 -9 8.92 0.50 1 -8 9 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0.68 4 -6 13 14.17 0.82 4 6 13 15.89 0.95 4 -6 -13 15.52 0.72 4 -6 -13 16.30 1.30 5 6 -13 13.62 0.81 5 -6 13 13.26 0.61 5 -6 13 14.61 0.76 -5 -6 -13 14.18 0.73 5 -6 -13 12.96 0.64 5 6 13 13.06 0.81 6 -6 13 5.82 0.42 6 -6 13 6.25 0.46 6 6 -13 6.03 0.45 6 -6 -13 6.48 0.34 6 6 13 6.41 0.52 0 -7 13 12.97 0.71 0 -7 -13 12.53 1.11 0 7 13 13.02 0.90 0 -7 13 12.50 0.61 1 -7 13 9.41 0.58 1 -7 13 10.40 0.68 -1 -7 -13 10.42 0.95 1 -7 13 9.99 0.53 1 -7 -13 10.28 0.95 1 7 13 10.39 0.80 -1 -7 13 10.04 0.61 2 -7 13 2.27 0.31 2 -7 13 2.46 0.26 -2 -7 13 2.74 0.30 2 -7 -13 2.65 0.49 2 7 13 2.88 0.44 3 -7 13 13.40 0.62 3 -7 13 13.61 0.74 3 7 13 12.59 0.86 -3 -7 13 13.49 0.73 3 -7 -13 12.86 0.63 3 -7 -13 12.99 1.14 4 -7 13 1.87 0.28 4 -7 13 1.91 0.22 4 7 -13 1.74 0.31 4 -7 -13 1.99 0.19 4 -7 -13 1.48 0.40 4 7 13 1.81 0.37 5 -7 13 20.20 0.82 5 7 -13 20.71 1.07 5 -7 13 22.31 1.00 5 -7 -13 20.88 0.90 5 7 13 20.83 1.13 6 -7 13 4.33 0.33 6 -7 13 4.41 0.31 6 7 -13 4.13 0.33 0 -8 -13 12.12 1.03 0 -8 13 11.47 0.64 0 -8 13 10.80 0.55 1 -8 13 6.04 0.41 -1 -8 -13 6.84 0.70 1 -8 13 6.55 0.39 1 -8 -13 5.49 0.67 -1 -8 13 5.43 0.41 2 -8 13 11.25 0.54 -2 -8 -13 11.28 0.95 2 -8 13 10.81 0.63 -2 -8 13 10.14 0.61 2 -8 -13 9.89 0.96 3 -8 13 13.98 0.61 3 -8 13 13.18 0.72 -3 -8 -13 13.53 1.09 -3 -8 13 14.18 0.73 3 -8 -13 13.91 0.64 3 -8 -13 13.35 1.15 4 -8 13 19.20 0.79 4 8 -13 20.10 1.02 -4 -8 -13 19.58 1.42 4 -8 13 19.64 0.95 4 8 13 21.97 1.12 4 -8 -13 18.61 1.50 4 -8 -13 21.13 0.87 5 8 -13 3.40 0.30 5 -8 13 2.69 0.33 5 -8 13 3.74 0.31 0 -9 -13 26.11 1.82 0 -9 13 25.43 1.15 0 -9 13 24.24 0.97 1 -9 13 3.43 0.28 1 -9 13 3.30 0.30 -1 -9 -13 3.63 0.50 1 -9 -13 4.42 0.54 -1 -9 13 4.44 0.34 2 -9 13 9.48 0.47 2 -9 13 9.12 0.55 -2 -9 -13 8.61 0.81 -2 -9 13 9.89 0.55 2 -9 -13 9.81 0.88 -3 -9 13 3.07 0.28 3 -9 -13 2.73 0.21 3 -9 -13 2.67 0.45 4 9 -13 11.00 0.60 4 -9 13 12.01 0.60 4 -9 -13 9.40 0.91 0 -10 13 0.00 0.09 0 -10 -13 0.01 0.10 0 -10 -13 0.04 0.17 1 -10 13 6.39 0.34 -1 -10 -13 6.56 0.61 1 -10 -13 5.36 0.61 -1 -10 13 5.54 0.38 -2 -10 -13 2.07 0.34 2 -10 13 2.06 0.19 2 -10 13 2.14 0.24 2 -10 -13 1.73 0.36 -2 -10 13 1.73 0.21 3 -10 13 4.81 0.34 3 -10 -13 4.82 0.59 0 -11 -13 28.40 1.18 -1 -11 -13 1.15 0.17 0 0 14 13.23 0.70 1 0 14 0.16 0.16 1 0 14 0.13 0.21 2 0 14 5.09 0.42 2 0 14 5.66 0.54 3 0 14 10.39 0.74 3 0 14 10.87 0.60 3 0 14 11.06 0.77 4 0 14 27.14 1.34 4 0 14 25.17 1.09 4 0 14 26.69 1.43 5 0 14 2.59 0.38 5 0 14 2.52 0.29 5 0 14 2.98 0.40 6 0 14 76.48 4.15 6 0 14 82.58 3.17 7 0 14 0.47 0.15 0 -1 14 1.26 0.24 0 1 14 1.23 0.25 1 -1 14 28.08 1.16 1 -1 14 27.14 1.36 1 1 14 28.09 1.18 1 1 14 26.92 1.41 2 -1 14 0.88 0.25 2 -1 14 0.54 0.18 2 1 14 0.45 0.19 2 1 14 0.58 0.26 2 1 14 0.48 0.21 3 -1 14 20.70 1.17 3 -1 14 19.40 1.07 3 -1 14 20.41 0.91 3 1 14 20.85 1.17 3 1 14 19.40 1.11 3 1 14 19.87 0.92 4 1 -14 8.70 0.66 4 -1 14 10.20 0.69 4 -1 14 9.78 0.57 4 -1 14 10.20 0.74 4 1 14 10.28 0.59 4 1 14 10.86 0.73 4 1 14 10.62 0.73 5 -1 14 17.89 0.95 5 -1 14 15.62 1.11 5 -1 14 17.41 0.77 5 -1 14 19.09 1.05 5 1 -14 16.63 0.95 5 1 14 17.87 1.03 5 1 14 16.23 0.77 5 1 14 16.08 0.94 6 -1 14 10.17 0.62 6 -1 14 9.03 0.68 6 1 -14 9.55 0.60 6 1 14 9.87 0.62 6 1 14 9.37 0.70 7 -1 14 2.82 0.28 7 1 -14 2.81 0.26 7 1 14 2.37 0.27 0 2 14 85.94 2.97 0 -2 14 82.71 2.90 1 -2 14 4.39 0.47 1 -2 14 4.05 0.37 1 2 14 4.38 0.51 1 2 14 4.17 0.40 2 -2 14 21.59 0.93 2 -2 14 21.28 1.12 2 2 14 20.25 0.96 2 2 14 20.54 1.16 2 2 14 20.26 1.17 3 -2 14 5.19 0.48 3 -2 14 4.40 0.46 3 -2 14 4.43 0.36 3 2 14 4.35 0.49 3 2 14 3.91 0.37 3 2 14 3.36 0.43 4 -2 14 0.14 0.17 4 2 -14 0.06 0.18 4 -2 14 0.27 0.16 4 -2 14 0.21 0.19 4 -2 14 -0.02 0.23 4 2 14 0.29 0.16 4 2 14 0.17 0.18 4 2 14 0.38 0.19 5 -2 14 7.21 0.58 5 -2 14 6.86 0.53 5 2 -14 6.54 0.53 5 -2 14 6.64 0.42 5 -2 14 6.99 0.62 5 2 14 7.02 0.45 5 2 14 7.40 0.58 5 2 14 7.57 0.58 6 -2 14 0.35 0.17 6 2 -14 0.47 0.18 6 -2 14 0.46 0.18 6 2 14 0.25 0.18 7 -2 14 0.11 0.11 7 2 -14 0.10 0.12 0 -3 14 10.81 0.60 0 3 14 11.27 0.66 1 -3 14 14.61 0.89 1 -3 14 15.57 0.76 1 3 14 16.88 1.01 1 3 14 17.45 0.84 2 -3 14 24.26 1.25 2 -3 14 25.90 1.07 2 3 14 26.24 1.13 2 3 14 25.18 1.34 2 3 14 25.75 1.37 3 -3 14 25.33 1.05 3 -3 14 25.21 1.25 3 -3 14 26.76 1.39 3 3 14 24.83 1.09 3 3 14 24.18 1.30 3 3 14 24.66 1.34 4 -3 14 0.21 0.17 4 -3 14 0.05 0.25 4 -3 14 0.23 0.14 4 3 -14 0.04 0.18 4 -3 14 0.06 0.17 4 3 14 0.14 0.19 4 3 14 0.11 0.15 4 3 14 0.22 0.18 5 -3 14 8.47 0.47 5 3 -14 8.07 0.60 5 -3 14 8.62 0.70 5 -3 14 8.89 0.59 5 -3 14 9.16 0.65 5 3 14 8.78 0.64 5 3 14 9.42 0.64 5 3 14 8.31 0.50 6 -3 14 0.59 0.18 6 3 -14 0.77 0.20 6 3 14 0.71 0.20 0 -4 14 17.26 0.79 0 4 14 17.54 0.87 0 -4 -14 16.90 1.36 1 -4 14 58.58 2.00 1 -4 14 58.05 2.42 1 4 14 54.79 2.47 1 4 14 53.84 2.06 1 -4 -14 51.27 3.60 2 -4 14 1.61 0.25 2 -4 14 1.39 0.28 2 4 14 1.77 0.29 2 4 14 1.88 0.37 3 -4 14 20.72 0.90 3 -4 14 22.04 1.09 3 -4 14 19.93 1.16 3 4 14 20.11 0.95 3 4 14 22.04 1.19 4 -4 14 9.47 0.62 4 -4 14 9.74 0.52 4 4 -14 9.31 0.66 4 -4 14 10.12 0.69 4 4 14 8.72 0.54 4 4 14 9.09 0.70 4 4 14 9.38 0.66 5 -4 14 0.80 0.16 5 4 -14 0.67 0.20 5 -4 14 0.61 0.19 5 -4 14 0.41 0.21 5 4 14 0.42 0.20 6 -4 14 16.55 0.98 6 -4 14 16.68 0.82 6 4 -14 17.04 0.89 6 4 14 16.17 0.85 0 5 14 9.25 0.59 0 -5 14 8.50 0.51 0 -5 -14 8.63 0.85 1 -5 14 0.95 0.19 1 5 14 0.76 0.21 1 -5 -14 0.55 0.27 1 5 14 0.44 0.26 2 -5 14 2.51 0.27 2 -5 14 2.55 0.34 2 5 14 2.57 0.32 2 -5 -14 2.18 0.44 2 5 14 2.47 0.43 3 -5 14 11.71 0.76 3 -5 14 10.74 0.68 3 -5 14 11.51 0.57 3 5 14 11.01 0.64 3 5 14 10.92 0.78 4 -5 14 1.78 0.24 4 -5 14 1.76 0.29 4 5 -14 1.58 0.30 4 5 14 1.43 0.31 4 5 14 1.83 0.28 5 5 -14 2.69 0.32 5 -5 14 2.08 0.33 5 -5 14 2.35 0.23 5 -5 14 2.20 0.30 5 -5 -14 3.14 0.22 5 5 14 3.04 0.37 6 -5 14 4.23 0.34 6 5 -14 4.16 0.35 6 -5 14 4.46 0.33 0 -6 14 19.66 0.84 0 6 14 18.72 1.14 0 -6 -14 20.19 1.51 1 -6 14 2.37 0.26 -1 -6 -14 2.37 0.44 1 -6 -14 2.36 0.45 1 6 14 2.45 0.44 1 6 14 2.56 0.34 2 -6 14 4.20 0.31 2 -6 14 4.40 0.40 2 6 14 3.03 0.45 2 6 14 3.52 0.37 2 -6 -14 2.84 0.48 3 -6 14 5.71 0.46 3 -6 14 5.60 0.38 3 -6 -14 6.63 0.69 3 6 14 6.39 0.57 4 -6 14 4.49 0.32 4 6 -14 4.40 0.40 4 -6 14 4.35 0.38 4 6 14 4.18 0.46 5 6 -14 23.97 1.21 5 -6 14 24.76 1.13 5 6 14 26.80 1.28 5 6 14 24.99 1.20 0 -7 14 7.46 0.43 0 -7 -14 8.05 0.79 -1 -7 -14 3.48 0.49 1 -7 14 3.51 0.28 1 7 14 2.98 0.46 1 -7 -14 3.09 0.49 2 -7 14 7.63 0.41 -2 -7 -14 7.50 0.71 2 -7 14 6.95 0.49 2 -7 -14 6.39 0.71 2 7 14 6.16 0.58 -3 -7 -14 4.21 0.48 3 -7 14 3.75 0.29 3 -7 14 3.67 0.34 3 7 14 3.46 0.42 3 -7 -14 3.34 0.49 4 7 -14 5.85 0.45 4 -7 14 6.46 0.37 -4 -7 -14 6.64 0.60 4 -7 14 6.09 0.43 4 7 14 6.08 0.52 5 -7 14 20.75 0.93 5 7 -14 19.65 0.98 0 -8 -14 20.15 1.50 -1 -8 -14 13.53 1.08 1 -8 14 12.85 0.59 1 -8 -14 13.93 1.11 2 -8 14 1.21 0.23 2 -8 14 1.18 0.18 -2 -8 -14 1.27 0.30 2 -8 -14 1.33 0.34 3 -8 14 8.95 0.44 -3 -8 -14 8.57 0.74 3 -8 14 8.52 0.51 3 -8 -14 8.59 0.80 4 -8 14 0.41 0.14 4 8 -14 0.38 0.14 0 -9 -14 0.77 0.25 -1 -9 -14 0.89 0.28 1 -9 14 0.82 0.15 1 -9 -14 1.10 0.29 2 -9 14 9.64 0.43 2 -9 14 8.14 0.49 -2 -9 -14 9.20 0.75 2 -9 -14 8.57 0.79 3 9 -14 1.91 0.22 3 -9 14 2.08 0.23 -1 -10 -14 1.49 0.19 0 0 15 0.13 0.16 1 0 15 18.51 0.85 1 0 15 17.80 1.02 2 0 15 24.85 1.32 2 0 15 26.74 1.12 2 0 15 28.79 1.43 3 0 15 0.53 0.22 3 0 15 0.55 0.17 3 0 15 0.56 0.23 4 0 15 17.12 0.78 4 0 15 14.80 0.90 4 0 15 18.69 1.00 5 0 15 8.41 0.47 5 0 15 9.54 0.60 6 0 15 0.58 0.17 6 0 15 0.46 0.16 0 1 15 0.96 0.23 0 -1 15 0.95 0.22 1 -1 15 4.01 0.46 1 -1 15 4.64 0.39 1 1 15 5.25 0.52 1 1 15 5.72 0.43 2 -1 15 3.62 0.44 2 -1 15 3.74 0.34 2 -1 15 3.85 0.42 2 1 15 4.21 0.47 2 1 15 4.07 0.42 2 1 15 4.16 0.37 3 -1 15 2.07 0.35 3 -1 15 1.92 0.27 3 -1 15 1.65 0.31 3 1 15 1.92 0.33 3 1 15 2.11 0.36 3 1 15 1.99 0.29 4 -1 15 6.27 0.52 4 -1 15 6.76 0.54 4 -1 15 6.42 0.43 4 1 15 6.93 0.55 4 1 15 6.95 0.55 4 1 15 7.19 0.46 5 -1 15 0.77 0.22 5 -1 15 1.01 0.18 5 -1 15 0.55 0.20 5 1 15 1.43 0.21 5 1 15 1.16 0.25 6 -1 15 0.18 0.14 6 -1 15 0.21 0.14 6 1 15 0.18 0.15 0 2 15 24.04 1.05 0 -2 15 23.47 1.01 1 -2 15 16.63 0.76 1 2 15 14.40 0.92 1 2 15 15.74 0.79 1 2 15 16.72 0.97 2 -2 15 15.67 0.71 2 -2 15 16.45 0.86 2 2 15 13.41 0.86 2 2 15 12.10 0.84 2 2 15 12.88 0.71 3 2 -15 8.18 0.59 3 -2 15 8.14 0.49 3 -2 15 7.69 0.60 3 -2 15 8.73 0.59 3 2 15 7.60 0.59 3 2 15 8.04 0.51 3 2 15 8.23 0.62 4 2 -15 5.26 0.46 4 -2 15 5.20 0.47 4 -2 15 6.95 0.53 4 -2 15 6.00 0.40 4 2 15 7.02 0.44 4 2 15 6.04 0.51 5 -2 15 15.43 0.80 5 -2 15 13.80 0.63 5 2 -15 14.52 0.79 5 -2 15 13.50 0.92 5 2 15 14.54 0.66 5 2 15 15.71 0.83 6 2 -15 2.60 0.28 6 -2 15 2.48 0.27 0 3 15 0.17 0.18 0 -3 15 0.30 0.15 1 -3 15 29.52 1.18 1 3 15 30.57 1.24 1 3 15 29.42 1.48 2 -3 15 14.39 0.70 2 -3 15 13.74 0.82 2 3 15 15.42 0.75 2 3 15 15.37 0.92 3 -3 15 0.62 0.21 3 -3 15 0.64 0.20 3 -3 15 0.70 0.17 3 3 15 0.54 0.22 3 3 15 0.68 0.20 3 3 15 0.72 0.23 4 3 -15 1.21 0.26 4 -3 15 0.98 0.18 4 -3 15 1.65 0.33 4 -3 15 1.28 0.26 4 3 15 1.29 0.28 4 3 15 1.04 0.21 5 -3 15 3.04 0.27 5 -3 15 2.22 0.31 5 3 -15 2.93 0.30 5 -3 15 2.79 0.31 5 3 15 2.28 0.33 6 -3 15 2.48 0.26 0 4 15 16.83 0.81 0 -4 -15 16.15 1.28 0 -4 15 16.35 0.75 1 -4 15 2.94 0.29 -1 -4 -15 2.84 0.44 1 4 15 3.16 0.44 1 4 15 2.94 0.34 2 -4 15 5.75 0.38 2 -4 15 5.12 0.45 2 4 15 5.31 0.54 2 4 15 5.11 0.42 3 -4 15 6.15 0.47 3 -4 15 6.32 0.39 3 -4 15 6.55 0.50 3 4 15 5.44 0.42 3 4 15 5.27 0.52 4 -4 15 8.03 0.53 4 4 -15 8.01 0.55 4 -4 15 8.55 0.45 4 4 15 8.14 0.48 4 4 15 7.82 0.59 5 -4 15 6.71 0.46 5 -4 15 6.82 0.52 5 4 -15 6.60 0.46 5 4 15 6.76 0.50 0 -5 15 6.71 0.42 0 -5 -15 6.87 0.70 0 5 15 7.24 0.50 -1 -5 -15 0.94 0.32 1 -5 15 1.04 0.19 1 -5 -15 0.50 0.25 1 5 15 0.71 0.20 1 5 15 0.54 0.24 2 -5 15 0.74 0.21 2 -5 15 0.76 0.17 2 5 15 0.93 0.22 2 5 15 0.93 0.27 3 -5 15 2.07 0.29 3 -5 15 1.72 0.38 3 -5 15 2.33 0.24 3 5 15 1.69 0.28 3 5 15 1.83 0.35 4 -5 15 2.46 0.24 4 -5 15 2.36 0.36 4 -5 15 2.25 0.28 4 5 -15 2.86 0.30 4 5 15 2.29 0.34 5 -5 15 3.91 0.35 5 -5 15 3.83 0.32 5 5 -15 3.88 0.32 0 -6 -15 4.16 0.52 1 -6 15 1.56 0.22 -1 -6 -15 1.69 0.35 1 6 15 1.20 0.30 1 -6 -15 1.01 0.32 -2 -6 -15 8.85 0.79 2 -6 15 8.80 0.46 2 -6 15 8.61 0.55 2 -6 -15 8.79 0.79 2 6 15 8.67 0.64 3 -6 15 4.72 0.39 3 -6 15 4.95 0.32 -3 -6 -15 5.02 0.52 3 6 15 4.74 0.46 4 -6 15 18.30 0.86 -4 -6 -15 18.62 1.28 4 -6 15 18.56 1.12 4 6 -15 18.08 0.91 4 6 15 15.84 0.90 0 -7 -15 6.03 0.63 1 -7 15 3.45 0.27 -1 -7 -15 3.60 0.46 1 -7 -15 3.76 0.47 2 -7 15 4.25 0.29 2 -7 15 4.18 0.35 -2 -7 -15 4.41 0.48 2 -7 -15 3.82 0.48 -3 -7 -15 0.02 0.14 3 -7 15 0.05 0.12 3 7 -15 0.00 0.11 3 -7 15 -0.03 0.21 4 -7 15 0.71 0.22 4 -7 15 0.88 0.18 0 -8 -15 3.08 0.41 -1 -8 -15 1.94 0.33 1 -8 -15 2.49 0.36 2 -8 15 2.35 0.37 0 0 16 60.19 2.13 1 0 16 8.59 0.61 1 0 16 9.30 0.53 2 0 16 20.16 1.08 2 0 16 22.30 0.93 2 0 16 22.51 1.17 3 0 16 8.34 0.48 3 0 16 8.65 0.59 4 0 16 4.00 0.38 4 0 16 3.40 0.30 5 0 16 1.53 0.26 0 1 16 0.55 0.19 0 1 16 0.42 0.18 0 -1 16 0.70 0.18 1 -1 16 8.41 0.50 1 1 16 8.28 0.62 1 1 16 8.83 0.61 1 1 16 9.12 0.53 2 -1 16 3.00 0.35 2 -1 16 3.22 0.30 2 -1 16 3.22 0.38 2 1 16 2.76 0.34 2 1 16 2.98 0.38 2 1 16 2.76 0.29 3 -1 16 6.57 0.51 3 -1 16 7.61 0.43 3 1 16 6.53 0.52 3 1 16 7.25 0.44 4 -1 16 1.22 0.26 4 -1 16 1.02 0.18 4 1 16 1.31 0.26 4 1 16 1.18 0.21 5 -1 16 1.89 0.25 5 1 16 1.50 0.26 0 -2 16 0.16 0.14 0 2 16 0.10 0.15 1 -2 16 9.73 0.52 1 2 16 8.85 0.53 1 2 16 8.99 0.65 2 -2 16 0.98 0.23 2 -2 16 1.18 0.25 2 -2 16 0.91 0.19 2 2 16 0.96 0.25 2 2 16 0.70 0.17 3 -2 16 2.35 0.32 3 -2 16 1.92 0.24 3 2 16 2.65 0.35 3 2 16 2.40 0.27 4 -2 16 9.31 0.46 4 -2 16 9.46 0.57 4 2 16 8.76 0.48 4 2 16 8.48 0.58 5 -2 16 0.42 0.16 0 3 16 1.50 0.26 -1 -3 -16 1.08 0.31 1 -3 16 1.39 0.22 1 3 16 1.55 0.26 1 3 16 1.65 0.34 2 -3 16 14.24 0.78 2 -3 16 14.72 0.66 2 3 16 14.09 0.69 2 3 16 13.39 0.83 3 3 -16 4.97 0.42 3 -3 16 6.25 0.37 3 -3 16 5.40 0.43 3 3 16 5.51 0.47 3 3 16 5.93 0.40 4 -3 16 0.57 0.18 4 3 -16 0.56 0.17 4 3 16 0.54 0.19 0 4 16 15.43 0.72 0 -4 -16 14.48 1.14 -1 -4 -16 6.22 0.63 1 -4 16 5.98 0.39 1 4 16 6.85 0.44 1 4 16 7.48 0.56 2 -4 16 14.15 0.77 2 -4 16 14.66 0.65 -2 -4 -16 14.81 1.11 2 4 16 13.85 0.83 2 4 16 15.53 0.70 3 -4 16 9.51 0.57 3 -4 16 9.17 0.47 3 4 -16 9.99 0.59 3 4 16 9.36 0.52 3 4 16 9.64 0.62 4 4 -16 0.54 0.15 4 -4 16 0.62 0.16 4 -4 16 0.44 0.18 4 4 16 0.60 0.19 0 -5 -16 0.86 0.27 1 -5 16 8.20 0.44 -1 -5 -16 8.31 0.73 1 5 16 8.00 0.58 -2 -5 -16 0.67 0.23 2 -5 16 0.79 0.18 2 -5 16 0.66 0.15 2 5 16 0.61 0.21 3 -5 16 12.63 0.67 -3 -5 -16 13.87 1.00 3 5 -16 12.01 0.70 3 5 16 13.96 0.75 0 -6 -16 0.03 0.15 -1 -6 -16 25.69 1.78 1 -6 -16 27.22 1.86 -2 -6 -16 1.32 0.29 2 -6 16 1.40 0.22 3 6 -16 2.42 0.24 1 0 17 11.10 0.55 2 0 17 2.34 0.31 2 0 17 3.04 0.26 3 0 17 6.76 0.47 1 -1 17 10.53 0.53 1 1 17 11.31 0.55 2 -1 17 2.68 0.25 2 -1 17 2.13 0.29 2 1 17 2.04 0.31 2 1 17 2.17 0.24 3 -1 17 2.61 0.29 3 1 17 2.37 0.30 1 -2 17 1.10 0.19 1 2 17 1.65 0.23 2 -2 17 8.12 0.51 2 2 17 7.79 0.53 3 -2 17 17.26 0.86 3 2 17 19.36 0.91 2 -3 17 6.03 0.42 2 3 17 5.54 0.44 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 7523 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 Br Br 0.42161(3) 0.52256(2) -0.03350(3) 0.03831(11) Uani 1 1 d S S 0.00130(7) 0.28449(5) 0.22027(5) 0.02664(16) Uani 1 1 d O1 O 0.1558(2) 0.20633(14) 0.06925(13) 0.0239(4) Uani 1 1 d O2 O -0.0271(2) 0.34713(16) 0.29531(15) 0.0339(5) Uani 1 1 d O3 O -0.1113(2) 0.25181(18) 0.16498(15) 0.0334(5) Uani 1 1 d N1 N 0.0781(3) 0.18655(17) 0.25671(16) 0.0232(5) Uani 1 1 d H1N H 0.094(4) 0.154(2) 0.212(3) 0.030(9) Uiso 1 1 d N2 N 0.3052(2) 0.07689(17) 0.20249(16) 0.0218(5) Uani 1 1 d C1 C 0.1194(3) 0.3497(2) 0.1514(2) 0.0270(6) Uani 1 1 d C2 C 0.1428(3) 0.4485(2) 0.1662(2) 0.0322(7) Uani 1 1 d H2 H 0.100(4) 0.476(3) 0.210(2) 0.027(8) Uiso 1 1 d C3 C 0.2328(4) 0.5008(2) 0.1119(2) 0.0353(8) Uani 1 1 d H3 H 0.239(4) 0.566(3) 0.121(3) 0.038(10) Uiso 1 1 d C4 C 0.2991(3) 0.4526(2) 0.0427(2) 0.0300(7) Uani 1 1 d C5 C 0.2778(3) 0.3538(2) 0.0251(2) 0.0273(6) Uani 1 1 d H5 H 0.321(4) 0.321(3) -0.026(3) 0.034(9) Uiso 1 1 d C6 C 0.1873(3) 0.3020(2) 0.0798(2) 0.0243(6) Uani 1 1 d C7 C 0.2486(3) 0.1432(2) 0.0195(2) 0.0248(6) Uani 1 1 d H7A H 0.204(3) 0.077(2) 0.025(2) 0.016(7) Uiso 1 1 d H7B H 0.253(3) 0.162(2) -0.046(2) 0.021(8) Uiso 1 1 d C8 C 0.3954(3) 0.1394(2) 0.05550(19) 0.0243(6) Uani 1 1 d H8A H 0.442(3) 0.079(2) 0.027(2) 0.024(8) Uiso 1 1 d H8B H 0.441(4) 0.195(3) 0.035(2) 0.032(9) Uiso 1 1 d C9 C 0.4105(3) 0.1390(2) 0.15833(19) 0.0242(6) Uani 1 1 d H9 H 0.395(3) 0.206(2) 0.179(2) 0.023(8) Uiso 1 1 d C10 C 0.5593(3) 0.1112(3) 0.1849(2) 0.0322(7) Uani 1 1 d H10A H 0.571(4) 0.125(2) 0.251(2) 0.030(9) Uiso 1 1 d H10B H 0.626(4) 0.155(2) 0.152(2) 0.032(9) Uiso 1 1 d C11 C 0.5873(3) 0.0023(3) 0.1701(2) 0.0354(7) Uani 1 1 d H11A H 0.680(4) -0.011(3) 0.191(3) 0.038(10) Uiso 1 1 d H11B H 0.590(4) -0.014(3) 0.107(3) 0.040(9) Uiso 1 1 d C12 C 0.4794(4) -0.0599(2) 0.2175(2) 0.0333(7) Uani 1 1 d H12A H 0.490(4) -0.052(2) 0.281(2) 0.030(9) Uiso 1 1 d H12B H 0.499(4) -0.131(3) 0.205(2) 0.027(8) Uiso 1 1 d C13 C 0.3344(3) -0.0281(2) 0.1889(2) 0.0261(6) Uani 1 1 d H13A H 0.320(3) -0.044(2) 0.121(2) 0.023(8) Uiso 1 1 d H13B H 0.267(4) -0.063(3) 0.223(2) 0.030(9) Uiso 1 1 d C14 C 0.2866(3) 0.1003(2) 0.2978(2) 0.0238(6) Uani 1 1 d H14A H 0.229(3) 0.048(2) 0.322(2) 0.023(8) Uiso 1 1 d H14B H 0.375(4) 0.107(2) 0.331(2) 0.030(9) Uiso 1 1 d C15 C 0.2053(3) 0.1959(2) 0.31178(19) 0.0218(6) Uani 1 1 d H15 H 0.267(3) 0.252(2) 0.291(2) 0.018(7) Uiso 1 1 d C16 C 0.1715(3) 0.2139(2) 0.41123(19) 0.0231(6) Uani 1 1 d H16 H 0.111(3) 0.263(2) 0.410(2) 0.019(8) Uiso 1 1 d C17 C 0.1023(3) 0.1272(2) 0.4561(2) 0.0315(7) Uani 1 1 d H17A H 0.071(4) 0.145(2) 0.515(2) 0.027(8) Uiso 1 1 d H17B H 0.169(4) 0.073(3) 0.463(3) 0.040(10) Uiso 1 1 d H17C H 0.015(5) 0.102(3) 0.420(3) 0.054(12) Uiso 1 1 d C18 C 0.2996(3) 0.2471(3) 0.4623(3) 0.0347(7) Uani 1 1 d H18A H 0.369(4) 0.195(3) 0.465(3) 0.043(10) Uiso 1 1 d H18B H 0.272(4) 0.261(3) 0.530(3) 0.036(9) Uiso 1 1 d H18C H 0.344(4) 0.305(3) 0.434(3) 0.042(11) Uiso 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br 0.02746(15) 0.02720(15) 0.0603(2) 0.01402(16) -0.00538(16) -0.00184(14) S 0.0223(3) 0.0345(4) 0.0231(3) 0.0000(3) -0.0027(3) 0.0086(3) O1 0.0222(10) 0.0247(9) 0.0248(10) -0.0010(8) 0.0016(8) -0.0007(8) O2 0.0359(12) 0.0391(12) 0.0268(11) -0.0040(9) -0.0029(9) 0.0159(10) O3 0.0207(10) 0.0505(12) 0.0291(11) 0.0017(10) -0.0047(9) 0.0052(9) N1 0.0211(11) 0.0288(12) 0.0198(11) -0.0012(10) 0.0001(10) 0.0048(12) N2 0.0195(11) 0.0239(12) 0.0219(12) -0.0002(10) 0.0043(10) -0.0018(9) C1 0.0255(14) 0.0297(15) 0.0257(15) 0.0014(12) -0.0091(12) 0.0056(12) C2 0.0342(16) 0.0299(16) 0.0326(18) -0.0012(13) -0.0099(15) 0.0133(14) C3 0.0389(17) 0.0225(15) 0.0445(19) 0.0030(13) -0.0158(16) 0.0039(13) C4 0.0267(14) 0.0262(14) 0.0370(17) 0.0074(13) -0.0118(14) 0.0011(11) C5 0.0249(13) 0.0285(13) 0.0286(16) 0.0046(13) -0.0039(14) 0.0028(12) C6 0.0219(13) 0.0251(14) 0.0259(15) 0.0031(12) -0.0066(12) 0.0025(11) C7 0.0246(14) 0.0295(14) 0.0202(15) -0.0027(12) 0.0031(12) -0.0025(12) C8 0.0226(15) 0.0256(14) 0.0247(15) 0.0003(11) 0.0054(11) -0.0031(12) C9 0.0216(13) 0.0270(14) 0.0240(14) -0.0007(11) 0.0030(12) -0.0029(13) C10 0.0213(14) 0.0485(19) 0.0268(16) 0.0000(14) 0.0016(13) -0.0049(14) C11 0.0228(14) 0.055(2) 0.0287(16) 0.0011(14) 0.0019(13) 0.0119(15) C12 0.0364(17) 0.0344(16) 0.0290(17) 0.0014(14) 0.0047(14) 0.0115(14) C13 0.0271(14) 0.0243(14) 0.0271(15) -0.0001(13) 0.0057(12) -0.0007(13) C14 0.0244(14) 0.0261(13) 0.0207(14) 0.0023(12) 0.0014(12) 0.0038(12) C15 0.0180(12) 0.0254(13) 0.0221(14) 0.0035(11) -0.0001(11) 0.0010(11) C16 0.0230(13) 0.0241(13) 0.0223(14) 0.0000(12) -0.0025(11) 0.0070(12) C17 0.0374(17) 0.0329(15) 0.0240(16) 0.0022(13) 0.0060(14) 0.0008(14) C18 0.0327(16) 0.0386(17) 0.0328(17) -0.0080(15) -0.0077(15) 0.0019(14) 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 S O3 119.23(13) O2 S N1 108.48(13) O3 S N1 106.43(14) O2 S C1 106.00(14) O3 S C1 108.09(14) N1 S C1 108.23(13) C6 O1 C7 119.7(2) C15 N1 S 119.6(2) C15 N1 H1N 110(3) S N1 H1N 105(2) C14 N2 C13 111.6(2) C14 N2 C9 113.0(2) C13 N2 C9 111.4(2) C2 C1 C6 119.6(3) C2 C1 S 120.0(3) C6 C1 S 120.4(2) C1 C2 C3 120.7(3) C1 C2 H2 118(2) C3 C2 H2 122(2) C4 C3 C2 118.9(3) C4 C3 H3 124(3) C2 C3 H3 117(3) C3 C4 C5 122.3(3) C3 C4 Br 119.8(2) C5 C4 Br 117.8(3) C4 C5 C6 118.5(3) C4 C5 H5 122(2) C6 C5 H5 120(2) O1 C6 C5 124.5(3) O1 C6 C1 115.4(3) C5 C6 C1 120.1(3) O1 C7 C8 114.7(2) O1 C7 H7A 103.5(17) C8 C7 H7A 109.8(17) O1 C7 H7B 111.6(18) C8 C7 H7B 108.4(19) H7A C7 H7B 109(2) C7 C8 C9 116.2(2) C7 C8 H8A 107.1(18) C9 C8 H8A 111.1(18) C7 C8 H8B 108(2) C9 C8 H8B 107(2) H8A C8 H8B 108(3) N2 C9 C10 112.7(2) N2 C9 C8 112.4(2) C10 C9 C8 110.3(2) N2 C9 H9 107.2(19) C10 C9 H9 107.0(19) C8 C9 H9 106.9(19) C11 C10 C9 111.6(3) C11 C10 H10A 107.7(19) C9 C10 H10A 108(2) C11 C10 H10B 113(2) C9 C10 H10B 109(2) H10A C10 H10B 107(3) C12 C11 C10 110.7(3) C12 C11 H11A 112(2) C10 C11 H11A 108(2) C12 C11 H11B 110(2) C10 C11 H11B 111(2) H11A C11 H11B 104(3) C11 C12 C13 109.9(3) C11 C12 H12A 109(2) C13 C12 H12A 110(2) C11 C12 H12B 108.7(19) C13 C12 H12B 113(2) H12A C12 H12B 106(3) N2 C13 C12 114.4(3) N2 C13 H13A 107.9(17) C12 C13 H13A 109.7(18) N2 C13 H13B 106(2) C12 C13 H13B 110(2) H13A C13 H13B 109(3) N2 C14 C15 112.2(2) N2 C14 H14A 105.9(19) C15 C14 H14A 106.2(19) N2 C14 H14B 113(2) C15 C14 H14B 107(2) H14A C14 H14B 112(3) N1 C15 C14 106.0(2) N1 C15 C16 111.8(2) C14 C15 C16 112.0(2) N1 C15 H15 112.0(17) C14 C15 H15 107.6(17) C16 C15 H15 107.4(17) C17 C16 C18 111.7(3) C17 C16 C15 113.2(3) C18 C16 C15 111.0(3) C17 C16 H16 108(2) C18 C16 H16 109(2) C15 C16 H16 104(2) C16 C17 H17A 110(2) C16 C17 H17B 110(2) H17A C17 H17B 108(3) C16 C17 H17C 112(2) H17A C17 H17C 107(3) H17B C17 H17C 109(3) C16 C18 H18A 111(2) C16 C18 H18B 109(2) H18A C18 H18B 106(3) C16 C18 H18C 112(2) H18A C18 H18C 107(3) H18B C18 H18C 112(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br C4 1.900(3) S O2 1.436(2) S O3 1.437(2) S N1 1.624(2) S C1 1.776(3) O1 C6 1.351(4) O1 C7 1.449(4) N1 C15 1.484(4) N1 H1N 0.82(4) N2 C14 1.470(4) N2 C13 1.476(4) N2 C9 1.479(4) C1 C2 1.386(4) C1 C6 1.413(4) C2 C3 1.387(5) C2 H2 0.86(4) C3 C4 1.381(5) C3 H3 0.91(4) C4 C5 1.389(4) C5 C6 1.390(4) C5 H5 0.97(4) C7 C8 1.518(4) C7 H7A 1.01(3) C7 H7B 1.01(3) C8 C9 1.542(4) C8 H8A 1.03(3) C8 H8B 0.93(4) C9 C10 1.539(4) C9 H9 0.97(3) C10 C11 1.528(5) C10 H10A 1.02(4) C10 H10B 1.01(4) C11 C12 1.520(5) C11 H11A 0.97(4) C11 H11B 0.97(4) C12 C13 1.528(4) C12 H12A 0.97(4) C12 H12B 1.01(3) C13 H13A 1.05(3) C13 H13B 0.96(4) C14 C15 1.537(4) C14 H14A 0.98(3) C14 H14B 1.00(4) C15 C16 1.540(4) C15 H15 1.03(3) C16 C17 1.516(4) C16 C18 1.523(4) C16 H16 0.88(3) C17 H17A 0.96(4) C17 H17B 0.99(4) C17 H17C 1.05(5) C18 H18A 0.98(4) C18 H18B 1.06(4) C18 H18C 1.00(4) 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 0.82(4) 2.33(4) 2.909(3) 129(3) . N1 H1N N2 0.82(4) 2.30(4) 2.778(3) 118(3) . C5 H5 O3 0.97(4) 2.40(4) 3.358(4) 169(3) 4 C7 H7A Br 1.01(3) 3.05(3) 3.893(3) 142(2) 4_455 C7 H7B O3 1.01(3) 2.50(3) 3.386(4) 146(2) 4 C13 H13B O2 0.96(4) 2.63(4) 3.433(4) 141(3) 3_545 C16 H16 Br 0.88(3) 3.07(3) 3.800(3) 142(2) 2_565 C16 H16 O2 0.88(3) 2.46(3) 3.160(4) 136(3) . 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 S N1 C15 -54.3(2) O3 S N1 C15 176.2(2) C1 S N1 C15 60.3(2) O2 S C1 C2 -12.8(3) O3 S C1 C2 116.1(2) N1 S C1 C2 -129.0(2) O2 S C1 C6 168.9(2) O3 S C1 C6 -62.2(3) N1 S C1 C6 52.7(3) C6 C1 C2 C3 -0.5(4) S C1 C2 C3 -178.8(2) C1 C2 C3 C4 0.0(5) C2 C3 C4 C5 0.6(5) C2 C3 C4 Br 179.4(2) C3 C4 C5 C6 -0.5(4) Br C4 C5 C6 -179.3(2) C7 O1 C6 C5 21.1(4) C7 O1 C6 C1 -159.9(2) C4 C5 C6 O1 178.9(3) C4 C5 C6 C1 0.0(4) C2 C1 C6 O1 -178.5(3) S C1 C6 O1 -0.2(3) C2 C1 C6 C5 0.5(4) S C1 C6 C5 178.8(2) C6 O1 C7 C8 57.3(3) O1 C7 C8 C9 39.0(4) C14 N2 C9 C10 74.1(3) C13 N2 C9 C10 -52.4(3) C14 N2 C9 C8 -160.6(2) C13 N2 C9 C8 72.9(3) C7 C8 C9 N2 40.3(4) C7 C8 C9 C10 166.9(2) N2 C9 C10 C11 53.2(3) C8 C9 C10 C11 -73.3(3) C9 C10 C11 C12 -53.7(3) C10 C11 C12 C13 53.8(3) C14 N2 C13 C12 -73.0(3) C9 N2 C13 C12 54.4(3) C11 C12 C13 N2 -55.2(4) C13 N2 C14 C15 -158.7(2) C9 N2 C14 C15 74.8(3) S N1 C15 C14 -154.0(2) S N1 C15 C16 83.6(3) N2 C14 C15 N1 51.2(3) N2 C14 C15 C16 173.4(2) N1 C15 C16 C17 66.9(3) C14 C15 C16 C17 -51.9(3) N1 C15 C16 C18 -166.5(2) C14 C15 C16 C18 74.6(3)