#------------------------------------------------------------------------------ #$Date: 2021-10-03 22:55:07 +0300 (Sun, 03 Oct 2021) $ #$Revision: 269492 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519070.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_4519070 loop_ _publ_author_name 'Laina-Mart\'in, V\'ictor' 'Humbr\'ias-Mart\'in, Jorge' 'Mas-Ballest\'e, Rub\'en' 'Fern\'andez-Salas, Jose A.' 'Alem\'an, Jos\'e' _publ_section_title ; Enantioselective Inverse-Electron Demand Aza-Diels--Alder Reaction: ipso,\a-Selectivity of Silyl Dienol Ethers ; _journal_issue 19 _journal_name_full 'ACS Catalysis' _journal_page_first 12133 _journal_page_last 12145 _journal_paper_doi 10.1021/acscatal.1c03390 _journal_volume 11 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_sum 'C31 H31 N O6.5 S' _chemical_formula_weight 553.63 _chemical_name_common VL_909_aftercol_250K _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.5571(2) _cell_length_b 12.9667(4) _cell_length_c 21.3679(6) _cell_measurement_reflns_used 8114 _cell_measurement_temperature 250.(2) _cell_measurement_theta_max 21.7759 _cell_measurement_theta_min 2.4701 _cell_volume 2925.07(13) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 250.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 36993 _diffrn_reflns_theta_full 25.34 _diffrn_reflns_theta_max 25.34 _diffrn_reflns_theta_min 3.13 _exptl_absorpt_coefficient_mu 0.156 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour 'clear colourless' _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.298 _exptl_crystal_size_mid 0.174 _exptl_crystal_size_min 0.094 _refine_diff_density_max 0.619 _refine_diff_density_min -0.250 _refine_ls_abs_structure_details ; Flack x determined using 1900 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 5339 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0483 _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^)+(0.0997P)^2^+0.9066P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1353 _refine_ls_wR_factor_ref 0.1444 _reflns_number_gt 4722 _reflns_number_total 5339 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c03390_si_002.cif _cod_data_source_block 03024DanielGonzalez _cod_original_formula_sum 'C31 H31 N O6.50 S' _cod_database_code 4519070 _shelx_res_file ; 03024_0m.res created by SHELXL-2014/7 TITL 03024_0m in P2(1)2(1)2(1) CELL 0.71073 10.55710 12.96670 21.36790 90.0000 90.0000 90.0000 ZERR 4.00 0.00020 0.00040 0.00060 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O S UNIT 124 124 4 26 4 OMIT 0 0 2 OMIT 1 0 1 OMIT 0 1 2 OMIT 0 1 1 OMIT 1 0 4 L.S. 60 ACTA BOND $H FMAP 2 PLAN 3 EADP C32 C29 EADP C18A C18B CONF EQIV $1 -x+1, y-1/2, -z+3/2 HTAB C9 O4_$1 HTAB C19 O5 HTAB C21 O6_$1 HTAB C32 O6 SIZE 0.094 0.174 0.298 DFIX 1.30 C17 C18A C17 C18B TEMP -23.130 WGHT 0.099700 0.906600 FVAR 0.17200 0.24794 PART 0 MOLE 1 C1 1 0.484443 0.498449 0.767570 11.00000 0.03227 0.03137 = 0.02926 0.00474 -0.00015 0.00064 C2 1 0.607163 0.522927 0.793052 11.00000 0.03477 0.03348 = 0.03522 0.00808 -0.00302 -0.00142 C3 1 0.655221 0.565038 0.848421 11.00000 0.04541 0.03944 = 0.04321 0.00220 -0.00555 -0.00567 AFIX 43 H3 2 0.600933 0.591569 0.879350 11.00000 -1.20000 AFIX 0 C4 1 0.785398 0.566360 0.856179 11.00000 0.05090 0.05454 = 0.05283 0.00736 -0.01966 -0.01212 AFIX 43 H4 2 0.819734 0.594382 0.893033 11.00000 -1.20000 AFIX 0 C5 1 0.866942 0.527063 0.810570 11.00000 0.03088 0.07471 = 0.06505 0.01384 -0.00692 -0.00842 AFIX 43 H5 2 0.954878 0.529116 0.817361 11.00000 -1.20000 AFIX 0 C6 1 0.821148 0.485576 0.756110 11.00000 0.03183 0.06575 = 0.05232 0.00718 0.00394 0.00292 AFIX 43 H6 2 0.875466 0.459449 0.725067 11.00000 -1.20000 AFIX 0 C7 1 0.690815 0.484104 0.749142 11.00000 0.03557 0.04483 = 0.03505 0.00952 -0.00168 -0.00297 C8 1 0.502066 0.447931 0.713455 11.00000 0.03131 0.03723 = 0.03129 0.00490 0.00364 0.00723 C9 1 0.409123 0.392633 0.674090 11.00000 0.03583 0.03275 = 0.03466 -0.00286 -0.00056 0.00513 AFIX 13 H9 2 0.425576 0.317757 0.678082 11.00000 -1.20000 AFIX 0 C10 1 0.416788 0.420785 0.605323 11.00000 0.03089 0.04127 = 0.03266 -0.00237 -0.00034 0.00135 C11 1 0.426118 0.346109 0.559589 11.00000 0.06598 0.04177 = 0.03992 -0.00749 -0.00203 0.00562 AFIX 43 H11 2 0.426672 0.276068 0.570931 11.00000 -1.20000 AFIX 0 C12 1 0.434734 0.373684 0.496674 11.00000 0.07480 0.06742 = 0.03415 -0.01463 -0.00001 0.00345 AFIX 43 H12 2 0.442832 0.322426 0.465824 11.00000 -1.20000 AFIX 0 C13 1 0.431391 0.475177 0.479955 11.00000 0.05332 0.07658 = 0.03033 0.00501 -0.00208 -0.00190 AFIX 43 H13 2 0.434986 0.493442 0.437420 11.00000 -1.20000 AFIX 0 C14 1 0.422955 0.549773 0.523995 11.00000 0.05568 0.05483 = 0.04809 0.01172 -0.00104 -0.00080 AFIX 43 H14 2 0.422434 0.619568 0.512107 11.00000 -1.20000 AFIX 0 C15 1 0.414998 0.522846 0.587322 11.00000 0.05265 0.03901 = 0.03603 -0.00342 -0.00263 0.00251 AFIX 43 H15 2 0.408380 0.574810 0.617821 11.00000 -1.20000 AFIX 0 C16 1 0.274357 0.414935 0.700813 11.00000 0.03314 0.03933 = 0.03683 -0.00361 -0.00126 0.00062 AFIX 13 H16 2 0.245264 0.481035 0.682618 11.00000 -1.20000 AFIX 0 C17 1 0.181157 0.333100 0.681459 11.00000 0.04768 0.07380 = 0.06382 -0.03218 0.00882 -0.01493 PART 1 AFIX 43 H17A 2 0.206451 0.292596 0.647182 21.00000 -1.20000 AFIX 43 PART 2 H17B 2 0.207804 0.264860 0.688324 -21.00000 -1.20000 AFIX 0 PART 1 C18A 1 0.076152 0.310798 0.703713 21.00000 0.04360 0.10257 = 0.08540 -0.03918 -0.01380 -0.00769 AFIX 93 H18A 2 0.044307 0.347864 0.738090 21.00000 -1.20000 H18B 2 0.028424 0.256830 0.686202 21.00000 -1.20000 AFIX 0 PART 2 C18B 1 0.075677 0.342117 0.658080 -21.00000 0.04360 0.10257 = 0.08540 -0.03918 -0.01380 -0.00769 AFIX 93 H18C 2 0.042644 0.408054 0.649841 -21.00000 -1.20000 H18D 2 0.027842 0.283094 0.648394 -21.00000 -1.20000 AFIX 0 PART 0 C19 1 0.273908 0.427161 0.771828 11.00000 0.03148 0.03117 = 0.04108 -0.00167 0.00281 -0.00089 AFIX 13 H19 2 0.186956 0.443282 0.786158 11.00000 -1.20000 AFIX 0 C20 1 0.245382 0.294667 0.847784 11.00000 0.05137 0.03864 = 0.04148 -0.00343 0.00837 -0.01387 C21 1 0.299250 0.194424 0.870422 11.00000 0.08322 0.04764 = 0.05897 0.01284 0.01628 -0.00552 AFIX 137 H21A 2 0.236768 0.140241 0.865252 11.00000 -1.50000 H21B 2 0.321464 0.200498 0.914316 11.00000 -1.50000 H21C 2 0.374374 0.177663 0.846346 11.00000 -1.50000 AFIX 0 C22 1 0.273188 0.682807 0.738981 11.00000 0.03636 0.02740 = 0.04179 -0.00279 -0.00121 0.00456 C23 1 0.154551 0.674233 0.711949 11.00000 0.03779 0.05356 = 0.06013 0.00461 -0.00531 0.00215 AFIX 43 H23 2 0.089099 0.638983 0.732732 11.00000 -1.20000 AFIX 0 C24 1 0.133583 0.718440 0.653691 11.00000 0.05598 0.06311 = 0.07243 -0.00188 -0.02758 0.01367 AFIX 43 H24 2 0.052851 0.713683 0.635362 11.00000 -1.20000 AFIX 0 C25 1 0.230319 0.769865 0.621824 11.00000 0.08339 0.04072 = 0.04650 0.00022 -0.01243 0.01726 C26 1 0.345836 0.778070 0.650773 11.00000 0.07064 0.03482 = 0.04377 -0.00145 0.00758 0.00344 AFIX 43 H26 2 0.411168 0.814238 0.630485 11.00000 -1.20000 AFIX 0 C27 1 0.369368 0.735063 0.708622 11.00000 0.04304 0.03232 = 0.03965 -0.00608 0.00256 -0.00008 AFIX 43 H27 2 0.449749 0.741193 0.727176 11.00000 -1.20000 AFIX 0 C28 1 0.204505 0.815190 0.559150 11.00000 0.14791 0.07249 = 0.05455 0.00863 -0.01970 0.03344 AFIX 137 H28A 2 0.284044 0.831258 0.538623 11.00000 -1.50000 H28B 2 0.155148 0.877784 0.563973 11.00000 -1.50000 H28C 2 0.157490 0.766080 0.533989 11.00000 -1.50000 AFIX 0 N1 3 0.361315 0.506020 0.795001 11.00000 0.03056 0.03219 = 0.03370 -0.00222 0.00449 -0.00072 O1 4 0.628182 0.438212 0.700038 11.00000 0.03087 0.05252 = 0.03657 0.00083 0.00286 0.00481 O2 4 0.314046 0.331029 0.798808 11.00000 0.04089 0.03279 = 0.04654 0.00550 0.01018 -0.00273 O3 4 0.156704 0.337274 0.869088 11.00000 0.06483 0.06725 = 0.07260 0.00514 0.03350 -0.00201 O4 4 0.402413 0.676408 0.841287 11.00000 0.05079 0.03808 = 0.04288 -0.00694 -0.00627 0.00053 O5 4 0.184842 0.605366 0.841666 11.00000 0.04779 0.04679 = 0.04903 -0.00443 0.01842 0.00334 S1 5 0.302609 0.622602 0.810831 11.00000 0.03682 0.03323 = 0.03330 -0.00333 0.00391 0.00142 MOLE 2 C29 1 0.768376 0.400626 0.551448 10.75000 0.04677 0.13196 = 0.06264 -0.00651 0.00482 0.00999 AFIX 137 H29A 2 0.755953 0.374564 0.593554 10.75000 -1.20000 H29B 2 0.766805 0.343657 0.522037 10.75000 -1.20000 H29C 2 0.701206 0.448843 0.541287 10.75000 -1.20000 AFIX 0 C30 1 0.888025 0.451945 0.547714 10.75000 0.06727 0.05532 = 0.07968 0.00061 -0.01769 0.01175 C31 1 1.090589 0.459301 0.499348 10.75000 0.04134 0.08518 = 0.08987 0.00645 0.00353 0.00835 AFIX 23 H31A 2 1.127968 0.472569 0.540549 10.75000 -1.20000 H31B 2 1.143912 0.408666 0.477779 10.75000 -1.20000 AFIX 0 C32 1 1.088229 0.552664 0.464201 10.75000 0.04677 0.13196 = 0.06264 -0.00651 0.00482 0.00999 AFIX 137 H32A 2 1.030311 0.601005 0.483729 10.75000 -1.20000 H32B 2 1.060199 0.538260 0.421862 10.75000 -1.20000 H32C 2 1.172571 0.582284 0.463084 10.75000 -1.20000 AFIX 0 O6 4 0.919128 0.524148 0.582132 10.75000 0.07322 0.11546 = 0.11136 -0.04811 -0.00001 0.01414 O7 4 0.959291 0.415641 0.507575 10.75000 0.06688 0.06145 = 0.04596 -0.00158 0.01016 -0.00923 HKLF 4 REM 03024_0m in P2(1)2(1)2(1) REM R1 = 0.0483 for 4722 Fo > 4sig(Fo) and 0.0567 for all 5339 data REM 372 parameters refined using 2 restraints END WGHT 0.0863 0.8369 REM Highest difference peak 0.619, deepest hole -0.250, 1-sigma level 0.061 Q1 1 0.9454 0.6018 0.5285 11.00000 0.05 0.62 Q2 1 0.9766 0.5146 0.5108 11.00000 0.05 0.58 Q3 1 0.7442 0.3299 0.5499 11.00000 0.05 0.56 ; _shelx_res_checksum 60681 _shelx_hkl_file ; 3 0 0 0.02 0.14 3 0 0 -0.07 0.16 3 0 0 -0.09 0.17 -3 0 0 -0.02 0.11 4 0 0 235.15 5.87 4 0 0 232.67 5.96 4 0 0 235.47 5.92 -4 0 0 231.52 5.77 4 0 0 235.28 5.74 5 0 0 -0.06 0.23 5 0 0 0.06 0.19 5 0 0 -0.02 0.14 -5 0 0 -0.04 0.15 5 0 0 -0.59 0.21 -6 0 0 15.40 0.68 6 0 0 15.73 0.71 -6 0 0 15.77 0.62 6 0 0 14.97 0.75 6 0 0 14.94 0.83 7 0 0 -0.16 0.27 -7 0 0 0.09 0.19 7 0 0 0.59 0.25 7 0 0 -0.14 0.25 -7 0 0 0.15 0.22 -8 0 0 15.06 0.74 8 0 0 15.22 0.85 8 0 0 13.84 0.91 8 0 0 14.44 0.78 -8 0 0 14.37 0.68 -9 0 0 -0.08 0.27 9 0 0 0.17 0.38 -9 0 0 0.21 0.30 9 0 0 0.31 0.31 9 0 0 -0.21 0.32 10 0 0 19.70 1.24 -10 0 0 19.68 1.24 10 0 0 19.22 1.02 -10 0 0 20.12 0.94 10 0 0 18.77 1.12 11 0 0 0.33 0.45 -11 0 0 -0.24 0.29 11 0 0 -0.11 0.32 11 0 0 -0.06 0.52 12 0 0 0.16 0.40 12 0 0 0.70 0.56 0 -1 0 0.04 0.05 2 -1 0 0.22 0.13 -2 -1 0 0.24 0.15 2 -1 0 0.18 0.12 2 -1 0 0.07 0.11 2 1 0 -0.13 0.14 2 -1 0 0.17 0.10 3 1 0 107.60 2.83 -3 -1 0 100.11 2.74 3 1 0 108.37 2.77 3 -1 0 109.35 2.70 3 -1 0 109.60 2.76 3 1 0 105.08 2.71 3 -1 0 106.10 2.81 3 -1 0 108.22 2.73 3 -1 0 105.94 2.76 3 1 0 107.57 2.84 4 1 0 2.97 0.36 4 -1 0 2.44 0.30 4 1 0 2.19 0.32 -4 1 0 2.66 0.15 4 1 0 3.02 0.32 4 -1 0 2.78 0.24 4 1 0 2.83 0.22 4 -1 0 2.97 0.32 -4 -1 0 3.61 0.41 4 -1 0 2.95 0.26 4 -1 0 2.43 0.32 -4 -1 0 2.35 0.28 5 -1 0 58.73 1.71 5 -1 0 57.54 1.60 5 -1 0 59.08 1.56 5 1 0 55.43 1.50 5 -1 0 57.23 1.69 -5 -1 0 59.17 1.71 5 -1 0 58.35 1.79 5 1 0 59.83 1.83 5 1 0 55.55 1.69 5 1 0 56.27 1.77 -5 1 0 55.93 1.49 -5 -1 0 55.89 1.64 6 -1 0 10.03 0.57 6 1 0 9.73 0.63 6 -1 0 8.56 0.64 6 -1 0 9.98 0.59 6 -1 0 9.52 0.47 -6 1 0 9.77 0.42 -6 -1 0 9.15 0.53 6 1 0 9.70 0.57 6 1 0 9.80 0.66 -6 -1 0 8.98 0.56 -7 -1 0 1.23 0.32 -7 1 0 0.66 0.19 7 -1 0 1.08 0.37 7 1 0 0.65 0.26 7 -1 0 0.77 0.27 7 -1 0 0.92 0.21 7 1 0 0.79 0.39 -7 -1 0 0.74 0.26 7 -1 0 1.43 0.35 7 1 0 1.75 0.40 8 -1 0 -0.30 0.32 8 -1 0 0.35 0.28 8 1 0 0.07 0.26 8 -1 0 0.20 0.17 8 -1 0 0.51 0.32 -8 -1 0 -0.24 0.28 8 1 0 -0.45 0.29 8 1 0 0.41 0.37 -8 1 0 0.22 0.22 -8 -1 0 0.02 0.26 -8 1 0 -0.07 0.19 -9 1 0 34.76 1.18 9 -1 0 34.77 1.56 9 1 0 35.01 1.48 9 -1 0 33.57 1.35 -9 -1 0 36.09 1.32 -9 1 0 33.46 1.23 9 -1 0 34.87 1.44 9 1 0 35.37 1.37 -9 -1 0 34.38 1.32 9 1 0 36.63 1.62 -10 -1 0 0.29 0.33 -10 -1 0 0.84 0.36 10 -1 0 0.69 0.37 10 1 0 0.92 0.44 10 1 0 0.67 0.37 -10 1 0 0.05 0.26 10 -1 0 0.45 0.41 10 -1 0 0.19 0.44 -11 -1 0 2.29 0.45 11 1 0 1.70 0.44 -11 -1 0 2.06 0.49 11 1 0 0.82 0.49 11 -1 0 1.32 0.57 11 -1 0 1.83 0.54 11 -1 0 1.78 0.46 12 -1 0 -0.35 0.48 12 -1 0 0.43 0.42 12 -1 0 -0.15 0.52 12 1 0 -0.42 0.45 12 1 0 0.76 0.42 2 -2 0 356.37 8.62 2 2 0 359.21 8.68 2 -2 0 359.49 8.65 2 -2 0 349.60 8.63 -2 -2 0 354.41 8.66 2 2 0 329.66 8.63 -2 -2 0 350.62 8.52 3 -2 0 35.19 1.03 3 -2 0 35.19 1.01 3 -2 0 33.64 1.07 -3 -2 0 33.18 1.10 3 -2 0 35.30 1.06 3 2 0 31.90 1.04 3 2 0 34.28 1.11 3 -2 0 34.89 1.06 -3 -2 0 33.02 1.08 4 -2 0 33.80 1.03 4 -2 0 33.11 1.04 4 -2 0 33.46 1.07 -4 -2 0 32.13 1.13 4 -2 0 33.31 1.09 4 -2 0 33.02 1.13 4 2 0 34.42 1.05 4 2 0 32.29 1.18 -4 -2 0 35.49 1.12 5 2 0 12.20 0.69 5 -2 0 13.66 0.59 5 -2 0 12.10 0.68 5 2 0 12.38 0.54 5 -2 0 11.80 0.60 -5 -2 0 12.43 0.63 5 2 0 12.79 0.62 5 -2 0 12.03 0.54 5 -2 0 12.29 0.58 -5 -2 0 13.03 0.66 -6 -2 0 4.77 0.49 -6 -2 0 5.30 0.47 6 2 0 4.99 0.46 6 -2 0 5.06 0.39 6 -2 0 5.75 0.49 6 2 0 5.68 0.56 6 -2 0 5.54 0.58 -6 2 0 5.01 0.24 6 -2 0 6.22 0.50 6 2 0 5.04 0.34 6 -2 0 4.91 0.41 7 -2 0 1.95 0.35 -7 -2 0 1.41 0.32 7 2 0 1.71 0.19 7 -2 0 1.95 0.30 7 2 0 1.69 0.35 7 2 0 2.24 0.47 -7 -2 0 1.56 0.35 7 -2 0 1.33 0.31 -7 2 0 1.74 0.19 7 -2 0 1.64 0.40 -8 2 0 0.29 0.17 -8 -2 0 0.28 0.32 8 2 0 0.29 0.27 8 2 0 0.25 0.38 8 -2 0 -0.10 0.20 8 -2 0 0.00 0.31 -8 -2 0 0.06 0.30 8 -2 0 0.12 0.25 8 -2 0 0.43 0.30 9 2 0 -0.33 0.38 9 -2 0 -0.24 0.28 -9 2 0 0.28 0.20 9 -2 0 0.21 0.39 9 -2 0 -0.53 0.20 -9 -2 0 -0.45 0.31 -9 -2 0 -0.10 0.32 9 -2 0 -0.19 0.31 9 2 0 -0.59 0.26 10 -2 0 7.59 0.76 -10 -2 0 8.04 0.71 10 -2 0 9.12 0.78 -10 2 0 8.36 0.55 10 2 0 10.14 0.82 -10 -2 0 8.06 0.73 10 -2 0 8.11 0.91 10 2 0 9.33 0.92 11 -2 0 0.64 0.40 11 2 0 2.28 0.60 -11 -2 0 0.12 0.38 11 -2 0 0.98 0.58 -11 -2 0 1.03 0.45 11 -2 0 0.32 0.39 11 2 0 0.58 0.39 12 -2 0 1.21 0.49 12 2 0 0.45 0.55 12 -2 0 0.43 0.51 12 2 0 -0.11 0.36 12 -2 0 0.39 0.44 -12 -2 0 -0.38 0.64 0 3 0 0.11 0.17 0 -3 0 0.01 0.18 0 -3 0 -0.21 0.19 0 -3 0 -0.24 0.17 1 -3 0 785.76 19.21 -1 3 0 805.99 19.36 1 -3 0 784.34 19.20 -1 -3 0 784.75 19.14 1 3 0 777.85 19.21 -1 -3 0 798.17 19.15 1 -3 0 781.39 19.19 -1 -3 0 801.89 19.50 -2 -3 0 24.83 0.75 -2 -3 0 25.04 0.88 2 3 0 23.41 0.85 2 -3 0 26.14 0.85 -2 -3 0 23.81 0.88 2 3 0 24.31 0.87 -2 -3 0 24.31 0.74 2 -3 0 24.54 0.86 2 -3 0 24.78 0.83 -3 -3 0 28.05 1.00 3 3 0 29.11 0.96 -3 -3 0 27.44 1.00 -3 -3 0 27.33 0.79 3 3 0 28.26 1.02 3 -3 0 26.64 0.96 3 -3 0 25.61 0.93 3 -3 0 28.05 0.94 3 -3 0 28.22 0.95 -3 -3 0 28.02 0.79 4 3 0 41.20 1.39 -4 -3 0 41.91 1.37 4 3 0 42.98 1.31 4 -3 0 40.12 1.27 -4 -3 0 42.40 1.36 4 -3 0 41.63 1.23 4 -3 0 40.65 1.31 4 -3 0 40.16 1.32 4 -3 0 40.78 1.31 5 3 0 52.15 1.75 5 -3 0 52.39 1.65 5 -3 0 52.66 1.70 -5 -3 0 51.42 1.70 -5 -3 0 53.60 1.69 5 -3 0 55.50 1.59 5 -3 0 53.37 1.59 5 -3 0 53.89 1.64 5 3 0 54.81 1.62 -6 -3 0 0.18 0.27 6 -3 0 0.07 0.23 6 3 0 0.22 0.32 -6 -3 0 0.22 0.29 6 -3 0 0.06 0.21 6 -3 0 0.26 0.28 6 3 0 0.25 0.20 6 3 0 -0.02 0.21 6 -3 0 -0.03 0.22 6 -3 0 -0.10 0.20 -7 -3 0 11.21 0.73 7 -3 0 11.10 0.69 7 -3 0 11.44 0.64 7 -3 0 13.11 0.64 7 3 0 11.93 0.71 7 3 0 12.39 0.86 7 3 0 11.93 0.58 7 -3 0 13.97 0.70 -7 3 0 12.06 0.41 7 -3 0 12.10 0.79 -7 -3 0 10.41 0.73 8 -3 0 0.11 0.33 8 -3 0 0.18 0.30 8 3 0 -0.26 0.16 8 -3 0 -0.12 0.25 8 -3 0 0.08 0.26 8 3 0 0.19 0.38 -8 -3 0 -0.53 0.29 -8 3 0 0.13 0.13 -8 -3 0 0.24 0.33 8 3 0 -0.14 0.26 9 3 0 16.07 1.05 -9 -3 0 18.66 1.01 -9 3 0 17.40 0.66 9 -3 0 17.86 0.85 9 -3 0 17.62 0.97 9 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22.28 0.92 3 -4 0 22.14 0.88 -3 -4 0 22.40 0.74 4 -4 0 46.78 1.50 -4 -4 0 45.90 1.57 -4 -4 0 46.21 1.31 4 4 0 49.09 1.54 -4 -4 0 48.05 1.30 4 4 0 48.24 1.61 4 -4 0 47.77 1.53 -4 -4 0 49.51 1.61 4 -4 0 48.00 1.52 4 -4 0 50.24 1.56 5 4 0 22.54 0.92 5 -4 0 22.89 0.95 5 -4 0 21.25 0.94 -5 -4 0 23.21 1.02 -5 -4 0 22.58 1.01 5 -4 0 23.85 0.95 5 4 0 22.16 1.01 5 -4 0 22.18 0.90 6 -4 0 0.18 0.24 6 -4 0 0.16 0.28 6 -4 0 0.18 0.21 -6 -4 0 0.42 0.30 6 4 0 0.50 0.33 -6 -4 0 0.32 0.29 6 4 0 -0.21 0.22 6 -4 0 0.52 0.29 6 -4 0 0.47 0.27 7 4 0 15.26 0.83 7 -4 0 15.77 0.78 7 -4 0 14.94 0.81 7 -4 0 14.89 0.86 7 -4 0 16.45 0.84 7 4 0 15.36 0.75 -7 -4 0 16.46 0.91 7 4 0 14.88 0.93 -7 -4 0 14.74 0.89 7 -4 0 15.62 0.75 -8 -4 0 53.66 1.92 8 -4 0 54.83 1.77 8 4 0 53.66 2.02 -8 4 0 53.39 1.43 8 -4 0 53.79 1.84 8 4 0 54.60 1.68 8 -4 0 53.55 1.73 -8 -4 0 50.78 1.88 8 -4 0 52.73 1.95 8 -4 0 54.15 1.81 8 4 0 51.21 1.83 -9 -4 0 20.29 1.11 9 -4 0 19.91 0.98 -9 4 0 19.23 0.68 9 -4 0 21.21 1.00 9 4 0 20.19 1.20 9 -4 0 19.76 1.04 9 4 0 19.76 0.80 9 -4 0 19.51 1.13 9 4 0 21.47 1.07 -9 -4 0 21.19 1.13 10 -4 0 4.59 0.75 -10 -4 0 4.13 0.64 10 -4 0 4.86 0.62 10 4 0 4.41 0.73 10 -4 0 5.03 0.65 10 -4 0 4.99 0.57 -10 -4 0 3.81 0.62 10 4 0 4.13 0.60 -11 -4 0 1.14 0.52 11 -4 0 1.51 0.50 11 -4 0 1.00 0.57 -11 -4 0 0.81 0.47 11 -4 0 1.45 0.63 11 4 0 0.84 0.45 11 4 0 1.23 0.57 12 -4 0 -0.61 0.47 -12 -4 0 0.06 0.48 12 4 0 -0.15 0.54 12 -4 0 0.21 0.41 -12 -4 0 -0.03 0.46 12 4 0 -0.12 0.41 0 -5 0 0.04 0.23 0 -5 0 0.18 0.22 0 -5 0 -0.05 0.20 0 -5 0 -0.30 0.23 0 5 0 0.25 0.22 1 5 0 23.54 0.90 1 -5 0 22.06 0.90 -1 -5 0 22.74 0.84 -1 -5 0 21.07 0.83 1 -5 0 23.57 0.88 -1 -5 0 23.16 0.89 1 -5 0 21.82 0.87 -1 -5 0 22.50 0.92 -1 5 0 21.42 0.82 -2 -5 0 0.90 0.31 2 -5 0 0.59 0.29 -2 -5 0 0.66 0.22 2 -5 0 1.07 0.32 -2 -5 0 0.93 0.30 -2 5 0 0.79 0.22 2 5 0 0.98 0.29 2 -5 0 0.91 0.24 2 -5 0 0.76 0.27 -2 -5 0 0.65 0.23 2 5 0 0.82 0.29 -3 -5 0 59.82 1.66 3 -5 0 57.46 1.84 3 -5 0 56.22 1.79 -3 -5 0 59.97 1.85 -3 -5 0 60.50 1.66 3 5 0 60.63 1.84 3 -5 0 54.91 1.78 -3 -5 0 54.72 1.83 -3 5 0 58.25 1.63 3 5 0 60.20 1.87 3 -5 0 58.13 1.75 4 5 0 10.65 0.70 4 5 0 9.84 0.62 4 -5 0 10.67 0.65 -4 -5 0 10.09 0.68 -4 -5 0 10.85 0.47 4 -5 0 10.23 0.60 -4 -5 0 9.99 0.66 4 -5 0 10.65 0.62 4 -5 0 10.48 0.66 -4 -5 0 10.89 0.49 -5 -5 0 -0.04 0.28 5 -5 0 0.27 0.29 -5 -5 0 0.07 0.35 -5 -5 0 -0.11 0.13 -5 -5 0 -0.06 0.14 5 5 0 0.27 0.32 5 -5 0 0.05 0.24 5 -5 0 0.08 0.27 5 -5 0 0.04 0.28 5 5 0 -0.10 0.23 6 5 0 11.49 0.69 6 -5 0 10.23 0.67 -6 -5 0 11.49 0.80 6 -5 0 10.87 0.72 6 5 0 11.55 0.81 6 -5 0 10.26 0.70 6 -5 0 12.10 0.74 -6 -5 0 11.41 0.79 7 5 0 7.65 0.78 -7 -5 0 9.22 0.81 7 -5 0 9.10 0.70 7 -5 0 7.63 0.70 7 5 0 8.79 0.62 7 -5 0 9.34 0.68 7 -5 0 9.42 0.69 -7 -5 0 7.90 0.77 8 -5 0 4.87 0.63 -8 -5 0 5.28 0.65 8 -5 0 5.19 0.56 8 5 0 4.63 0.51 -8 -5 0 4.94 0.64 8 5 0 4.85 0.72 8 5 0 5.56 0.65 8 -5 0 5.10 0.62 8 -5 0 5.29 0.62 -9 -5 0 38.78 1.67 9 5 0 41.88 1.62 9 -5 0 39.38 1.60 9 -5 0 39.14 1.56 9 5 0 38.35 1.77 9 -5 0 39.12 1.72 -9 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0.29 3 -6 0 2.08 0.34 4 -6 0 22.28 0.96 4 6 0 24.59 1.05 4 -6 0 23.12 1.04 4 -6 0 21.78 0.99 4 -6 0 23.71 1.03 -4 6 0 22.63 0.81 -4 -6 0 23.53 1.08 -4 -6 0 23.91 0.85 4 6 0 22.17 1.08 -4 -6 0 23.20 0.83 -4 -6 0 23.02 1.07 -5 -6 0 42.70 1.29 5 -6 0 42.96 1.53 5 6 0 44.26 1.67 5 -6 0 43.15 1.58 5 -6 0 42.22 1.54 -5 -6 0 43.38 1.27 -5 -6 0 42.94 1.61 5 -6 0 42.19 1.50 -5 -6 0 42.06 1.60 5 6 0 46.33 1.58 6 6 0 6.22 0.60 6 -6 0 6.72 0.62 6 -6 0 6.58 0.65 6 -6 0 6.81 0.68 -6 -6 0 5.97 0.70 6 -6 0 8.28 0.72 -6 -6 0 5.91 0.68 6 6 0 5.16 0.68 -7 -6 0 5.81 0.69 7 -6 0 3.46 0.49 7 -6 0 5.05 0.62 7 -6 0 3.74 0.54 7 6 0 4.09 0.53 -7 -6 0 3.39 0.55 7 6 0 3.34 0.63 7 -6 0 3.39 0.55 8 -6 0 4.67 0.64 8 6 0 5.04 0.58 -8 -6 0 5.47 0.75 8 -6 0 7.03 0.75 8 6 0 4.24 0.71 8 -6 0 4.14 0.61 8 -6 0 5.04 0.61 -8 -6 0 5.57 0.74 9 -6 0 0.71 0.37 9 6 0 -0.24 0.34 -9 -6 0 1.08 0.50 9 -6 0 0.25 0.39 -9 -6 0 0.47 0.47 9 -6 0 -0.40 0.33 9 6 0 -0.14 0.53 9 -6 0 0.24 0.36 10 -6 0 0.74 0.40 10 -6 0 0.12 0.46 10 -6 0 -0.06 0.38 -10 -6 0 0.32 0.52 -10 -6 0 0.25 0.48 10 6 0 1.20 0.62 10 6 0 -0.01 0.39 11 -6 0 0.15 0.51 11 6 0 -0.13 0.41 -11 -6 0 0.17 0.50 11 6 0 0.81 0.63 11 -6 0 0.29 0.38 -11 -6 0 0.65 0.55 11 -6 0 -0.25 0.42 0 -7 0 0.48 0.26 0 -7 0 -0.01 0.28 0 -7 0 -0.16 0.24 0 7 0 0.11 0.25 0 -7 0 0.02 0.25 -1 7 0 52.60 1.68 1 7 0 54.14 1.75 1 -7 0 52.11 1.62 1 -7 0 50.97 1.72 -1 -7 0 51.25 1.69 -1 -7 0 50.75 1.70 1 -7 0 54.95 1.79 -1 -7 0 50.99 1.70 -1 -7 0 51.69 1.73 -2 -7 0 16.12 0.80 -2 -7 0 17.22 0.80 2 7 0 17.75 0.90 2 -7 0 17.43 0.88 -2 7 0 17.10 0.78 2 -7 0 16.79 0.78 2 -7 0 18.19 0.93 -2 -7 0 18.07 0.88 2 7 0 18.87 0.92 2 -7 0 17.79 0.73 -2 -7 0 17.47 0.93 3 7 0 7.86 0.66 -3 -7 0 5.07 0.57 -3 -7 0 6.77 0.53 -3 -7 0 7.10 0.66 3 -7 0 6.46 0.62 3 -7 0 6.91 0.67 3 -7 0 8.07 0.62 -3 -7 0 6.29 0.51 3 7 0 6.68 0.66 -3 7 0 6.91 0.49 -4 -7 0 29.46 1.05 4 7 0 30.45 1.26 -4 7 0 29.53 1.03 4 7 0 29.76 1.29 -4 -7 0 29.25 1.26 4 -7 0 27.59 1.24 4 -7 0 27.45 1.22 -4 -7 0 28.67 1.03 -4 -7 0 31.32 1.30 4 -7 0 29.95 1.23 4 -7 0 28.41 1.14 5 -7 0 9.89 0.73 -5 -7 0 9.39 0.52 5 7 0 10.10 0.73 -5 -7 0 9.91 0.54 5 7 0 12.56 0.85 5 -7 0 11.59 0.86 -5 7 0 10.39 0.54 5 -7 0 9.60 0.67 -5 -7 0 10.20 0.84 -5 -7 0 9.91 0.83 5 -7 0 11.10 0.78 6 7 0 1.25 0.47 -6 -7 0 0.69 0.40 6 -7 0 0.50 0.38 6 -7 0 0.78 0.37 -6 -7 0 1.08 0.44 6 -7 0 1.32 0.41 -6 -7 0 0.78 0.21 6 -7 0 0.47 0.32 6 7 0 1.11 0.41 -6 -7 0 1.00 0.26 7 -7 0 21.49 1.08 -7 -7 0 19.65 1.14 7 -7 0 17.39 1.08 -7 -7 0 21.53 1.23 7 7 0 19.61 1.20 7 -7 0 17.73 1.03 7 -7 0 17.76 1.05 7 7 0 18.15 1.20 8 7 0 3.05 0.69 -8 -7 0 5.30 0.75 -8 -7 0 3.40 0.64 8 -7 0 3.44 0.57 8 -7 0 3.22 0.61 8 -7 0 2.34 0.52 8 -7 0 3.61 0.60 -9 -7 0 -0.34 0.41 9 -7 0 0.15 0.40 -9 -7 0 0.16 0.49 9 -7 0 -0.09 0.39 9 7 0 0.04 0.39 9 -7 0 -0.84 0.32 9 7 0 -0.19 0.54 9 -7 0 0.27 0.39 10 7 0 -0.20 0.40 -10 -7 0 -0.45 0.48 10 -7 0 0.39 0.45 -10 -7 0 0.84 0.57 10 7 0 0.99 0.66 10 -7 0 -0.45 0.36 10 -7 0 0.33 0.43 11 7 0 1.11 0.51 11 7 0 0.96 0.63 -11 -7 0 1.23 0.61 11 -7 0 0.05 0.47 11 -7 0 1.35 0.49 -11 -7 0 0.69 0.58 11 -7 0 0.15 0.50 0 -8 0 17.32 0.85 0 -8 0 17.28 0.91 0 -8 0 17.58 0.89 0 8 0 17.43 0.90 0 -8 0 16.87 0.84 1 -8 0 6.01 0.63 1 -8 0 4.86 0.48 1 8 0 5.07 0.56 -1 -8 0 5.95 0.56 1 8 0 5.00 0.54 -1 -8 0 6.67 0.63 -1 -8 0 8.53 0.71 1 -8 0 5.90 0.60 -1 -8 0 5.71 0.57 -1 8 0 5.94 0.54 2 -8 0 1.78 0.36 2 -8 0 1.24 0.40 -2 -8 0 1.93 0.39 2 8 0 1.76 0.42 -2 8 0 1.25 0.33 -2 -8 0 1.69 0.39 2 -8 0 0.30 0.33 -2 -8 0 2.11 0.44 2 8 0 1.70 0.39 2 -8 0 1.77 0.32 -2 -8 0 2.03 0.41 3 8 0 20.30 1.04 -3 -8 0 20.43 0.92 -3 -8 0 20.78 0.92 -3 -8 0 21.33 1.06 3 -8 0 19.72 1.06 3 -8 0 21.61 1.07 3 8 0 19.57 1.02 3 -8 0 21.31 0.94 -3 -8 0 21.28 1.07 -3 8 0 20.73 0.90 3 -8 0 22.15 1.06 -4 -8 0 0.22 0.34 -4 -8 0 -0.15 0.25 4 -8 0 -0.31 0.29 -4 -8 0 0.12 0.23 4 -8 0 0.10 0.25 4 8 0 0.43 0.37 -4 -8 0 0.10 0.35 -4 8 0 0.19 0.23 4 -8 0 -0.21 0.35 -5 -8 0 10.45 0.93 5 -8 0 10.26 0.92 -5 -8 0 11.19 0.62 5 8 0 11.18 0.97 -5 8 0 11.68 0.64 -5 -8 0 10.78 0.92 -5 -8 0 12.00 0.64 5 -8 0 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-2 -23 2.91 0.68 2 -2 23 2.62 0.66 -2 2 23 2.61 0.49 2 -2 -23 2.00 0.59 -2 2 -23 2.58 0.71 2 -2 -23 2.06 0.72 2 -2 -23 2.16 0.53 -2 -2 23 3.16 0.52 2 2 23 2.26 0.61 3 2 -23 -0.29 0.39 -3 -2 -23 0.35 0.42 3 -2 23 1.53 0.61 -3 -2 -23 1.20 0.60 -3 -2 -23 0.92 0.60 -3 2 -23 1.06 0.59 3 -2 -23 0.67 0.55 3 -2 -23 0.76 0.50 3 -2 -23 0.99 0.50 3 2 23 0.85 0.54 4 2 -23 1.37 0.53 -4 -2 -23 2.31 0.70 4 -2 23 1.97 0.69 -4 -2 -23 1.05 0.64 4 -2 -23 0.18 0.58 4 -2 -23 0.72 0.51 4 2 23 2.16 0.67 -4 2 -23 1.40 0.63 4 -2 -23 1.52 0.49 -5 -2 -23 1.39 0.65 5 2 -23 0.13 0.38 -5 -2 -23 0.89 0.60 5 -2 23 0.97 0.64 5 2 -23 0.88 0.49 5 2 -23 0.83 0.55 5 2 23 -0.33 0.47 -5 2 -23 -0.18 0.54 5 -2 -23 0.52 0.57 5 -2 -23 0.93 0.54 0 -3 -23 5.05 0.89 0 3 -23 5.20 0.84 0 -3 23 4.97 0.73 0 3 23 5.64 0.75 0 -3 -23 5.11 0.77 0 -3 -23 4.83 0.70 -1 -3 -23 1.79 0.56 -1 -3 -23 1.75 0.62 -1 3 23 2.97 0.58 1 -3 23 1.45 0.58 1 3 -23 2.34 0.62 -1 -3 -23 3.09 0.74 1 -3 -23 2.91 0.74 -1 -3 23 2.00 0.53 1 -3 -23 3.26 0.63 1 3 23 2.63 0.63 -1 3 -23 2.08 0.69 1 -3 -23 1.23 0.54 -2 -3 -23 4.91 0.84 -2 -3 -23 4.44 0.87 -2 -3 -23 5.50 0.73 -2 3 23 4.79 0.62 2 -3 23 3.36 0.70 2 3 -23 3.26 0.71 2 -3 -23 4.28 0.71 -2 3 -23 5.30 0.91 2 -3 -23 5.22 0.91 2 -3 -23 4.64 0.70 2 3 23 4.34 0.77 -2 -3 23 5.04 0.62 3 3 -23 4.16 0.74 -3 -3 -23 3.00 0.76 3 -3 23 3.97 0.80 -3 -3 -23 3.17 0.77 -3 3 -23 2.79 0.77 3 -3 -23 4.08 0.66 3 -3 -23 3.14 0.74 3 3 23 3.63 0.78 3 -3 -23 3.29 0.64 4 3 -23 0.84 0.53 4 -3 23 1.04 0.61 -4 -3 -23 0.25 0.57 -4 -3 -23 1.05 0.64 4 -3 -23 1.46 0.57 -4 3 -23 0.98 0.59 4 -3 -23 0.53 0.43 4 -3 -23 1.59 0.65 4 3 23 1.44 0.67 5 3 -23 -0.18 0.42 5 -3 23 0.61 0.56 -5 -3 -23 0.32 0.62 -5 -3 -23 -0.33 0.52 5 3 23 -0.45 0.48 5 -3 -23 0.10 0.49 5 -3 -23 0.02 0.53 -5 3 -23 0.35 0.54 0 -4 23 1.98 0.55 0 4 -23 0.63 0.58 0 -4 -23 1.54 0.54 0 -4 -23 1.46 0.59 0 -4 -23 0.98 0.62 0 4 23 1.25 0.54 -1 -4 -23 2.35 0.59 -1 4 23 2.47 0.56 -1 -4 -23 2.54 0.75 -1 -4 -23 2.72 0.70 1 4 -23 2.34 0.65 1 -4 23 1.81 0.58 1 4 23 2.25 0.62 1 -4 -23 2.10 0.60 -1 -4 23 1.62 0.50 -1 4 -23 1.37 0.61 1 -4 -23 2.18 0.68 1 -4 -23 2.13 0.59 -2 -4 -23 1.48 0.62 2 -4 23 0.97 0.53 -2 -4 -23 0.69 0.50 -2 -4 -23 -0.16 0.46 2 4 -23 0.16 0.46 -2 4 23 0.32 0.41 -2 -4 23 0.45 0.40 -2 4 -23 -0.43 0.46 2 -4 -23 0.92 0.47 2 -4 -23 0.96 0.52 2 4 23 0.46 0.52 2 -4 -23 1.40 0.67 -3 -4 -23 11.29 1.17 3 4 -23 11.46 1.11 -3 -4 -23 12.48 1.24 3 -4 23 11.76 1.20 3 4 23 10.88 1.13 3 -4 -23 10.48 1.05 -3 4 -23 11.70 1.22 3 -4 -23 11.91 1.24 3 -4 -23 13.30 0.99 4 4 -23 0.25 0.49 4 -4 23 0.52 0.58 -4 -4 -23 -0.32 0.51 -4 -4 -23 0.25 0.59 4 4 23 -0.24 0.54 4 -4 -23 0.61 0.62 4 -4 -23 0.18 0.43 -4 4 -23 0.58 0.62 4 -4 -23 0.27 0.53 0 -5 23 -0.13 0.42 0 -5 -23 -0.30 0.39 0 -5 -23 -0.03 0.56 0 -5 -23 -0.10 0.45 0 5 23 0.14 0.47 0 5 -23 -0.35 0.51 -1 5 23 4.93 0.73 1 -5 23 4.81 0.75 -1 -5 -23 3.66 0.77 -1 -5 -23 5.04 0.90 -1 -5 -23 4.11 0.77 1 5 -23 3.88 0.82 -1 5 -23 5.04 0.86 1 -5 -23 5.07 0.82 -1 -5 23 4.06 0.66 1 5 23 6.02 0.84 1 -5 -23 4.36 0.90 1 -5 -23 4.87 0.77 -2 -5 -23 2.17 0.63 -2 5 23 2.30 0.55 -2 -5 -23 3.02 0.76 2 -5 23 1.47 0.62 2 5 -23 2.82 0.73 -2 -5 -23 1.39 0.67 2 5 23 2.33 0.69 2 -5 -23 2.78 0.78 -2 5 -23 2.93 0.78 2 -5 -23 2.92 0.71 2 -5 -23 1.30 0.53 -2 -5 23 2.90 0.56 3 5 -23 3.04 0.73 -3 -5 -23 2.43 0.71 -3 -5 -23 1.78 0.72 3 -5 23 2.71 0.71 3 5 23 2.22 0.66 -3 5 -23 2.87 0.81 3 -5 -23 2.71 0.68 3 -5 -23 2.75 0.79 3 -5 -23 2.79 0.56 -4 -5 -23 4.12 0.88 4 -5 23 3.10 0.78 -4 -5 -23 3.26 0.79 4 5 -23 3.58 0.74 -4 5 -23 2.15 0.71 4 -5 -23 3.53 0.80 4 5 23 3.65 0.86 4 -5 -23 2.85 0.75 0 -6 -23 1.74 0.63 0 -6 23 2.10 0.59 0 -6 -23 1.93 0.70 0 6 -23 1.61 0.65 0 -6 -23 2.23 0.68 0 6 23 1.81 0.59 -1 -6 -23 1.46 0.60 1 -6 23 2.25 0.64 1 6 -23 2.00 0.64 -1 6 23 2.12 0.60 -1 -6 -23 2.10 0.69 -1 -6 -23 2.40 0.75 1 -6 -23 2.44 0.69 1 6 23 2.37 0.69 1 -6 -23 2.09 0.60 -1 6 -23 2.87 0.72 -1 -6 23 2.36 0.59 1 -6 -23 2.48 0.75 -2 -6 -23 1.76 0.68 2 -6 23 3.93 0.78 -2 6 23 2.68 0.58 2 6 -23 3.04 0.71 -2 -6 -23 2.29 0.76 2 -6 -23 2.39 0.70 2 -6 -23 2.79 0.78 -2 6 -23 1.85 0.66 2 6 23 2.40 0.70 2 -6 -23 2.57 0.60 -2 -6 23 3.67 0.65 0 -7 -23 0.75 0.61 0 -7 -23 0.40 0.62 0 7 23 1.04 0.53 0 -7 -23 0.33 0.51 0 -7 23 1.02 0.53 0 7 -23 -0.71 0.46 0 0 24 1.24 0.48 0 0 -24 1.47 0.57 1 0 -24 -0.88 0.40 -1 0 24 0.08 0.41 -1 0 -24 0.38 0.56 1 0 -24 -0.19 0.47 1 0 24 0.30 0.47 2 0 -24 2.42 0.70 2 0 -24 1.61 0.61 2 0 24 1.77 0.62 -2 0 -24 2.28 0.68 3 0 -24 0.31 0.43 3 0 -24 0.79 0.43 3 0 -24 0.69 0.58 3 0 24 0.80 0.55 -3 0 -24 0.48 0.54 4 0 24 3.28 0.73 4 0 -24 3.08 0.72 4 0 -24 3.45 0.63 -4 0 -24 3.14 0.80 4 0 -24 3.42 0.64 0 -1 -24 4.24 0.81 0 1 24 5.91 0.74 0 1 -24 4.04 0.80 0 -1 -24 4.54 0.79 0 -1 24 5.37 0.73 -1 -1 -24 1.52 0.64 -1 1 24 3.09 0.59 -1 -1 -24 1.58 0.71 1 1 -24 2.72 0.70 1 -1 24 2.38 0.62 1 -1 -24 2.79 0.69 -1 1 -24 3.88 0.76 1 -1 -24 3.10 0.70 1 -1 -24 2.01 0.50 -1 -1 24 2.00 0.54 1 1 24 2.48 0.61 -2 -1 -24 1.18 0.65 -2 -1 -24 2.14 0.73 2 -1 24 0.95 0.52 2 1 -24 -0.13 0.45 2 -1 -24 0.68 0.49 2 1 24 1.25 0.56 2 -1 -24 0.96 0.45 -2 1 -24 0.15 0.58 2 -1 -24 0.25 0.57 3 1 -24 -0.49 0.47 3 1 -24 0.00 0.42 -3 -1 -24 0.39 0.52 3 -1 24 0.25 0.55 3 -1 -24 -0.09 0.45 -3 1 -24 0.23 0.60 3 -1 -24 0.35 0.53 3 -1 -24 -0.19 0.36 3 1 24 0.11 0.52 4 1 -24 3.11 0.64 4 -1 24 2.51 0.72 -4 -1 -24 3.03 0.81 4 1 -24 2.81 0.70 4 -1 -24 3.39 0.64 4 -1 -24 3.53 0.68 4 1 24 3.40 0.77 4 -1 -24 3.35 0.74 -4 1 -24 5.47 0.93 0 2 -24 0.19 0.55 0 -2 -24 -0.03 0.51 0 -2 -24 -0.34 0.49 0 -2 24 -0.35 0.40 0 2 24 0.31 0.43 0 -2 -24 0.35 0.40 -1 -2 -24 0.90 0.56 -1 -2 -24 0.59 0.42 -1 -2 -24 0.64 0.53 1 -2 24 -0.64 0.40 1 2 -24 -0.01 0.53 -1 2 24 0.10 0.40 -1 2 -24 0.10 0.54 1 -2 -24 -0.06 0.47 1 -2 -24 -0.77 0.49 -1 -2 24 0.10 0.39 1 -2 -24 0.52 0.42 1 2 24 0.57 0.51 2 -2 24 2.11 0.64 -2 -2 -24 2.49 0.75 2 2 -24 1.35 0.62 -2 -2 -24 1.38 0.68 2 2 24 1.95 0.61 2 -2 -24 0.62 0.46 2 -2 -24 2.14 0.61 2 -2 -24 1.65 0.64 -2 2 -24 2.01 0.71 -3 -2 -24 2.30 0.70 3 2 -24 1.84 0.60 3 -2 24 2.42 0.70 -3 -2 -24 1.71 0.71 3 -2 -24 3.30 0.65 3 2 24 1.68 0.63 3 -2 -24 1.51 0.55 3 -2 -24 1.96 0.69 -3 2 -24 2.40 0.69 -4 -2 -24 0.10 0.53 4 2 -24 0.60 0.54 4 -2 24 0.81 0.62 -4 -2 -24 0.05 0.55 4 2 -24 0.72 0.50 4 2 24 -0.01 0.54 4 -2 -24 0.73 0.50 -4 2 -24 1.15 0.65 4 -2 -24 1.04 0.45 4 -2 -24 0.37 0.59 0 -3 -24 1.91 0.70 0 -3 -24 0.45 0.46 0 -3 -24 0.42 0.54 0 -3 24 0.46 0.46 0 3 24 -0.63 0.37 0 3 -24 0.30 0.54 -1 -3 -24 0.40 0.55 -1 3 24 0.46 0.43 1 -3 24 -0.15 0.43 1 3 -24 0.90 0.58 -1 -3 -24 0.29 0.42 -1 -3 -24 -0.23 0.52 1 -3 -24 0.40 0.59 1 3 24 0.50 0.48 -1 3 -24 -0.20 0.46 1 -3 -24 0.17 0.44 1 -3 -24 0.71 0.49 -1 -3 24 -0.19 0.36 -2 -3 -24 1.88 0.70 -2 -3 -24 1.54 0.54 2 -3 24 2.33 0.66 -2 -3 -24 0.82 0.63 2 3 -24 1.70 0.58 -2 3 -24 1.19 0.60 2 3 24 1.81 0.62 2 -3 -24 2.12 0.57 2 -3 -24 1.60 0.65 2 -3 -24 1.46 0.52 -3 -3 -24 2.91 0.79 3 3 -24 3.14 0.68 -3 -3 -24 3.76 0.67 3 -3 24 2.78 0.73 -3 -3 -24 3.61 0.80 3 -3 -24 2.85 0.78 3 3 24 3.44 0.75 3 -3 -24 2.31 0.57 -3 3 -24 2.99 0.80 3 -3 -24 3.26 0.68 0 4 -24 7.70 0.98 0 -4 24 5.81 0.79 0 -4 -24 6.72 1.01 0 4 24 6.48 0.84 0 -4 -24 6.11 0.82 0 -4 -24 6.01 0.89 -1 -4 -24 1.30 0.56 1 4 -24 0.40 0.58 -1 4 24 0.18 0.43 -1 -4 -24 0.67 0.56 -1 -4 -24 0.97 0.62 1 -4 24 0.68 0.53 1 -4 -24 0.89 0.54 -1 -4 24 -0.03 0.41 1 -4 -24 -0.39 0.61 -1 4 -24 1.80 0.72 1 -4 -24 1.07 0.53 1 4 24 1.22 0.57 2 -4 24 6.15 0.89 -2 -4 -24 5.01 0.94 2 4 -24 6.80 0.93 -2 4 24 7.96 0.79 -2 -4 -24 7.34 0.98 -2 -4 -24 7.09 0.86 -2 4 -24 6.46 0.99 2 -4 -24 6.37 0.83 2 -4 -24 5.90 0.84 -2 -4 24 6.64 0.73 2 -4 -24 8.12 1.05 2 4 24 5.60 0.88 -3 -4 -24 0.90 0.62 -3 -4 -24 -0.19 0.54 3 -4 24 0.14 0.50 3 4 -24 -0.31 0.41 3 -4 -24 0.72 0.54 -3 4 -24 -0.46 0.54 3 -4 -24 0.60 0.62 3 -4 -24 0.30 0.44 3 4 24 -0.88 0.49 0 -5 -24 1.36 0.74 0 5 24 1.31 0.55 0 -5 -24 1.37 0.61 0 -5 24 0.73 0.49 0 5 -24 -0.21 0.52 0 -5 -24 1.24 0.59 1 -5 24 1.80 0.59 -1 -5 -24 0.52 0.53 -1 -5 -24 0.49 0.52 -1 -5 -24 0.28 0.64 -1 5 24 0.87 0.52 1 5 -24 0.73 0.63 1 5 24 0.58 0.55 -1 5 -24 0.76 0.56 1 -5 -24 0.23 0.52 -1 -5 24 1.04 0.51 1 -5 -24 1.54 0.59 1 -5 -24 1.89 0.71 -2 -5 -24 1.51 0.61 -2 5 24 1.93 0.55 -2 -5 -24 1.01 0.64 -2 -5 -24 1.58 0.69 2 -5 24 1.74 0.65 2 5 -24 1.78 0.68 -2 -5 24 0.72 0.45 2 -5 -24 1.40 0.73 -2 5 -24 0.91 0.59 2 5 24 0.52 0.56 2 -5 -24 1.44 0.55 2 -5 -24 0.91 0.57 0 0 25 1.28 0.52 0 0 -25 0.55 0.54 1 0 -25 0.05 0.51 -1 0 -25 0.05 0.50 -1 0 25 0.44 0.44 1 0 -25 0.19 0.57 1 0 25 -0.22 0.46 2 0 25 3.28 0.74 -2 0 -25 2.80 0.73 2 0 -25 1.51 0.57 2 0 -25 2.13 0.75 3 0 -25 1.48 0.55 3 0 25 0.89 0.61 3 0 -25 1.32 0.62 -3 0 -25 1.31 0.66 0 1 25 0.12 0.45 0 -1 -25 -0.41 0.49 0 1 -25 1.33 0.57 0 -1 25 0.05 0.43 0 -1 -25 0.05 0.54 1 1 -25 2.95 0.71 -1 -1 -25 3.08 0.76 -1 1 25 3.40 0.61 1 -1 25 2.23 0.64 -1 -1 -25 2.92 0.74 -1 -1 25 2.95 0.61 1 -1 -25 4.39 0.78 1 -1 -25 2.60 0.73 1 1 25 3.26 0.67 -1 1 -25 3.95 0.83 2 -1 25 1.64 0.62 -2 -1 -25 0.67 0.66 2 1 -25 1.17 0.61 -2 -1 -25 1.05 0.65 2 -1 -25 0.96 0.55 2 -1 -25 1.15 0.46 2 1 25 1.61 0.60 -2 1 -25 2.52 0.71 2 -1 -25 0.04 0.59 0 2 -25 5.31 0.87 0 -2 -25 5.54 0.91 0 2 25 5.91 0.78 0 -2 -25 4.67 0.81 0 -2 25 4.89 0.75 0 -2 -25 4.72 0.68 -1 -2 -25 0.70 0.62 -1 -2 -25 -0.15 0.51 1 2 -25 -0.40 0.50 -1 2 25 0.92 0.46 1 -2 25 -0.49 0.45 -1 -2 25 0.37 0.42 1 -2 -25 1.12 0.48 1 2 25 1.35 0.53 -1 2 -25 -0.26 0.55 1 -2 -25 -0.40 0.54 1 -2 -25 0.55 0.56 -2 -2 -25 0.78 0.63 2 -2 25 2.15 0.69 -2 -2 -25 1.94 0.71 2 2 -25 2.39 0.68 -2 2 -25 1.06 0.62 2 -2 -25 2.74 0.65 2 2 25 0.94 0.57 2 -2 -25 2.19 0.57 2 -2 -25 1.86 0.71 0 -3 -25 0.48 0.46 0 -3 25 1.30 0.52 0 -3 -25 0.44 0.58 0 3 -25 0.49 0.52 0 3 25 -0.30 0.44 0 -3 -25 1.11 0.60 -1 -3 -25 -0.01 0.61 -1 -3 -25 0.48 0.44 -1 3 25 1.07 0.49 1 -3 25 0.57 0.53 1 3 -25 -0.01 0.53 -1 -3 -25 1.60 0.61 1 -3 -25 -0.15 0.44 1 -3 -25 0.13 0.50 1 3 25 0.74 0.51 1 -3 -25 -0.06 0.51 -1 -3 25 0.67 0.44 -1 3 -25 0.46 0.57 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 89276 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_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.4844(3) 0.4984(3) 0.76757(17) 0.0310(8) Uani d . . . 1.0 . . C C2 0.6072(4) 0.5229(3) 0.79305(18) 0.0345(8) Uani d . . . 1.0 . . C C3 0.6552(4) 0.5650(3) 0.8484(2) 0.0427(10) Uani d . . . 1.0 . . H H3 0.6009 0.5916 0.8794 0.051 Uiso calc U . R 1.0 . . C C4 0.7854(5) 0.5664(4) 0.8562(2) 0.0528(12) Uani d . . . 1.0 . . H H4 0.8197 0.5944 0.893 0.063 Uiso calc U . R 1.0 . . C C5 0.8669(4) 0.5271(4) 0.8106(3) 0.0569(12) Uani d . . . 1.0 . . H H5 0.9549 0.5291 0.8174 0.068 Uiso calc U . R 1.0 . . C C6 0.8211(4) 0.4856(4) 0.7561(2) 0.0500(11) Uani d . . . 1.0 . . H H6 0.8755 0.4594 0.7251 0.06 Uiso calc U . R 1.0 . . C C7 0.6908(4) 0.4841(3) 0.74914(18) 0.0385(9) Uani d . . . 1.0 . . C C8 0.5021(3) 0.4479(3) 0.71345(17) 0.0333(8) Uani d . . . 1.0 . . C C9 0.4091(4) 0.3926(3) 0.67409(17) 0.0344(8) Uani d . . . 1.0 . . H H9 0.4256 0.3178 0.6781 0.041 Uiso calc U . R 1.0 . . C C10 0.4168(4) 0.4208(3) 0.60532(18) 0.0349(8) Uani d . . . 1.0 . . C C11 0.4261(5) 0.3461(3) 0.5596(2) 0.0492(11) Uani d . . . 1.0 . . H H11 0.4267 0.2761 0.5709 0.059 Uiso calc U . R 1.0 . . C C12 0.4347(5) 0.3737(5) 0.4967(2) 0.0588(13) Uani d . . . 1.0 . . H H12 0.4428 0.3224 0.4658 0.071 Uiso calc U . R 1.0 . . C C13 0.4314(5) 0.4752(4) 0.4800(2) 0.0534(12) Uani d . . . 1.0 . . H H13 0.435 0.4934 0.4374 0.064 Uiso calc U . R 1.0 . . C C14 0.4230(5) 0.5498(4) 0.5240(2) 0.0529(11) Uani d . . . 1.0 . . H H14 0.4224 0.6196 0.5121 0.063 Uiso calc U . R 1.0 . . C C15 0.4150(4) 0.5228(3) 0.58732(19) 0.0426(10) Uani d . . . 1.0 . . H H15 0.4084 0.5748 0.6178 0.051 Uiso calc U . R 1.0 . . C C16 0.2744(4) 0.4149(3) 0.70081(18) 0.0364(9) Uani d . . . 1.0 . . H H16 0.2453 0.481 0.6826 0.044 Uiso calc U . R 1.0 . . C C17 0.1812(5) 0.3331(5) 0.6815(3) 0.0618(14) Uani d . . D 1.0 . . H H17A 0.2065 0.2926 0.6472 0.074 Uiso calc U P R 0.248(12) A 1 H H17B 0.2078 0.2649 0.6883 0.074 Uiso calc U P R 0.752(12) A 2 C C18A 0.0762(18) 0.311(2) 0.7037(14) 0.077(3) Uani d . P D 0.248(12) A 1 H H18A 0.0443 0.3479 0.7381 0.093 Uiso calc U P R 0.248(12) A 1 H H18B 0.0284 0.2568 0.6862 0.093 Uiso calc U P R 0.248(12) A 1 C C18B 0.0757(7) 0.3421(8) 0.6581(4) 0.077(3) Uani d . P D 0.752(12) A 2 H H18C 0.0426 0.4081 0.6498 0.093 Uiso calc U P R 0.752(12) A 2 H H18D 0.0278 0.2831 0.6484 0.093 Uiso calc U P R 0.752(12) A 2 C C19 0.2739(3) 0.4272(3) 0.77183(19) 0.0346(8) Uani d . . . 1.0 . . H H19 0.187 0.4433 0.7862 0.041 Uiso calc U . R 1.0 . . C C20 0.2454(5) 0.2947(3) 0.8478(2) 0.0438(10) Uani d . . . 1.0 . . C C21 0.2992(6) 0.1944(4) 0.8704(3) 0.0633(14) Uani d . . . 1.0 . . H H21A 0.2368 0.1402 0.8653 0.095 Uiso calc U . R 1.0 . . H H21B 0.3215 0.2005 0.9143 0.095 Uiso calc U . R 1.0 . . H H21C 0.3744 0.1777 0.8463 0.095 Uiso calc U . R 1.0 . . C C22 0.2732(4) 0.6828(3) 0.73898(19) 0.0352(9) Uani d . . . 1.0 . . C C23 0.1546(4) 0.6742(4) 0.7119(2) 0.0505(11) Uani d . . . 1.0 . . H H23 0.0891 0.639 0.7327 0.061 Uiso calc U . R 1.0 . . C C24 0.1336(5) 0.7184(4) 0.6537(3) 0.0638(14) Uani d . . . 1.0 . . H H24 0.0529 0.7137 0.6354 0.077 Uiso calc U . R 1.0 . . C C25 0.2303(6) 0.7699(4) 0.6218(2) 0.0569(13) Uani d . . . 1.0 . . C C26 0.3458(5) 0.7781(3) 0.6508(2) 0.0497(11) Uani d . . . 1.0 . . H H26 0.4112 0.8142 0.6305 0.06 Uiso calc U . R 1.0 . . C C27 0.3694(4) 0.7351(3) 0.70862(19) 0.0383(9) Uani d . . . 1.0 . . H H27 0.4497 0.7412 0.7272 0.046 Uiso calc U . R 1.0 . . C C28 0.2045(8) 0.8152(5) 0.5591(3) 0.092(2) Uani d . . . 1.0 . . H H28A 0.284 0.8313 0.5386 0.137 Uiso calc U . R 1.0 . . H H28B 0.1551 0.8778 0.564 0.137 Uiso calc U . R 1.0 . . H H28C 0.1575 0.7661 0.534 0.137 Uiso calc U . R 1.0 . . N N1 0.3613(3) 0.5060(2) 0.79500(14) 0.0321(7) Uani d . . . 1.0 . . O O1 0.6282(2) 0.4382(2) 0.70004(13) 0.0400(7) Uani d . . . 1.0 . . O O2 0.3140(3) 0.3310(2) 0.79881(13) 0.0401(6) Uani d . . . 1.0 . . O O3 0.1567(4) 0.3373(3) 0.86909(19) 0.0682(10) Uani d . . . 1.0 . . O O4 0.4024(3) 0.6764(2) 0.84129(14) 0.0439(7) Uani d . . . 1.0 . . O O5 0.1848(3) 0.6054(2) 0.84167(14) 0.0479(7) Uani d . . . 1.0 . . S S1 0.30261(9) 0.62260(7) 0.81083(4) 0.0344(3) Uani d . . . 1.0 . . C C29 0.7684(7) 0.4006(8) 0.5514(4) 0.0805(18) Uani d . P . 0.75 . . H H29A 0.756 0.3746 0.5936 0.097 Uiso calc U P R 0.75 . . H H29B 0.7668 0.3437 0.522 0.097 Uiso calc U P R 0.75 . . H H29C 0.7012 0.4488 0.5413 0.097 Uiso calc U P R 0.75 . . C C30 0.8880(8) 0.4519(6) 0.5477(4) 0.067(2) Uani d . P . 0.75 . . C C31 1.0906(7) 0.4593(7) 0.4993(4) 0.072(2) Uani d . P . 0.75 . . H H31A 1.128 0.4726 0.5405 0.087 Uiso calc U P R 0.75 . . H H31B 1.1439 0.4087 0.4778 0.087 Uiso calc U P R 0.75 . . C C32 1.0882(7) 0.5527(8) 0.4642(4) 0.0805(18) Uani d . P . 0.75 . . H H32A 1.0303 0.601 0.4837 0.097 Uiso calc U P R 0.75 . . H H32B 1.0602 0.5383 0.4219 0.097 Uiso calc U P R 0.75 . . H H32C 1.1726 0.5823 0.4631 0.097 Uiso calc U P R 0.75 . . O O6 0.9191(6) 0.5241(6) 0.5821(3) 0.100(2) Uani d . P . 0.75 . . O O7 0.9593(5) 0.4156(4) 0.5076(2) 0.0581(12) Uani d . P . 0.75 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0323(19) 0.0314(19) 0.0293(18) 0.0006(15) -0.0002(15) 0.0047(15) C2 0.0348(19) 0.0335(18) 0.0352(19) -0.0014(16) -0.0030(16) 0.0081(16) C3 0.045(2) 0.039(2) 0.043(2) -0.0057(18) -0.0055(19) 0.0022(18) C4 0.051(3) 0.055(3) 0.053(3) -0.012(2) -0.020(2) 0.007(2) C5 0.031(2) 0.075(3) 0.065(3) -0.008(2) -0.007(2) 0.014(3) C6 0.032(2) 0.066(3) 0.052(3) 0.003(2) 0.0039(19) 0.007(2) C7 0.036(2) 0.045(2) 0.035(2) -0.0030(18) -0.0017(17) 0.0095(16) C8 0.0313(18) 0.037(2) 0.0313(18) 0.0072(16) 0.0036(15) 0.0049(15) C9 0.0358(19) 0.0328(19) 0.0347(19) 0.0051(16) -0.0006(16) -0.0029(15) C10 0.0309(19) 0.041(2) 0.033(2) 0.0013(16) -0.0003(15) -0.0024(16) C11 0.066(3) 0.042(2) 0.040(2) 0.006(2) -0.002(2) -0.0075(18) C12 0.075(3) 0.067(3) 0.034(2) 0.003(3) 0.000(2) -0.015(2) C13 0.053(3) 0.077(3) 0.030(2) -0.002(3) -0.002(2) 0.005(2) C14 0.056(3) 0.055(3) 0.048(3) -0.001(2) -0.001(2) 0.012(2) C15 0.053(3) 0.039(2) 0.036(2) 0.003(2) -0.0026(19) -0.0034(17) C16 0.033(2) 0.0393(19) 0.037(2) 0.0006(15) -0.0013(16) -0.0036(16) C17 0.048(3) 0.074(3) 0.064(3) -0.015(2) 0.009(2) -0.032(3) C18A 0.044(3) 0.103(6) 0.085(6) -0.008(4) -0.014(4) -0.039(5) C18B 0.044(3) 0.103(6) 0.085(6) -0.008(4) -0.014(4) -0.039(5) C19 0.031(2) 0.0312(18) 0.041(2) -0.0009(15) 0.0028(16) -0.0017(16) C20 0.051(2) 0.039(2) 0.041(2) -0.014(2) 0.008(2) -0.0034(18) C21 0.083(4) 0.048(3) 0.059(3) -0.006(3) 0.016(3) 0.013(2) C22 0.036(2) 0.0274(17) 0.042(2) 0.0046(16) -0.0012(17) -0.0028(16) C23 0.038(2) 0.054(3) 0.060(3) 0.002(2) -0.005(2) 0.005(2) C24 0.056(3) 0.063(3) 0.072(3) 0.014(3) -0.028(3) -0.002(3) C25 0.083(4) 0.041(2) 0.046(3) 0.017(2) -0.012(3) 0.000(2) C26 0.071(3) 0.035(2) 0.044(2) 0.003(2) 0.008(2) -0.0014(18) C27 0.043(2) 0.0323(19) 0.040(2) -0.0001(17) 0.0026(18) -0.0061(16) C28 0.148(7) 0.072(4) 0.055(3) 0.033(4) -0.020(4) 0.009(3) N1 0.0306(15) 0.0322(16) 0.0337(16) -0.0007(13) 0.0045(13) -0.0022(13) O1 0.0309(13) 0.0525(16) 0.0366(15) 0.0048(12) 0.0029(12) 0.0008(12) O2 0.0409(15) 0.0328(13) 0.0465(16) -0.0027(12) 0.0102(13) 0.0055(12) O3 0.065(2) 0.067(2) 0.073(2) -0.0020(19) 0.0335(19) 0.0051(19) O4 0.0508(17) 0.0381(15) 0.0429(15) 0.0005(13) -0.0063(13) -0.0069(13) O5 0.0478(17) 0.0468(17) 0.0490(16) 0.0033(14) 0.0184(14) -0.0044(14) S1 0.0368(5) 0.0332(4) 0.0333(5) 0.0014(4) 0.0039(4) -0.0033(4) C29 0.047(3) 0.132(6) 0.063(3) 0.010(3) 0.005(2) -0.007(3) C30 0.067(5) 0.055(4) 0.080(5) 0.012(4) -0.018(4) 0.001(4) C31 0.041(3) 0.085(5) 0.090(6) 0.008(4) 0.004(4) 0.006(5) C32 0.047(3) 0.132(6) 0.063(3) 0.010(3) 0.005(2) -0.007(3) O6 0.073(4) 0.115(5) 0.111(5) 0.014(4) 0.000(4) -0.048(4) O7 0.067(3) 0.061(3) 0.046(2) -0.009(2) 0.010(2) -0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C8 C1 N1 . . 120.9(3) ? C8 C1 C2 . . 108.0(3) ? N1 C1 C2 . . 130.4(3) ? C7 C2 C3 . . 119.0(4) ? C7 C2 C1 . . 103.7(3) ? C3 C2 C1 . . 137.1(4) ? C4 C3 C2 . . 117.8(4) ? C4 C3 H3 . . 121.1 ? C2 C3 H3 . . 121.1 ? C3 C4 C5 . . 121.6(4) ? C3 C4 H4 . . 119.2 ? C5 C4 H4 . . 119.2 ? C6 C5 C4 . . 121.2(4) ? C6 C5 H5 . . 119.4 ? C4 C5 H5 . . 119.4 ? C5 C6 C7 . . 116.6(4) ? C5 C6 H6 . . 121.7 ? C7 C6 H6 . . 121.7 ? O1 C7 C2 . . 111.6(3) ? O1 C7 C6 . . 124.5(4) ? C2 C7 C6 . . 123.8(4) ? C1 C8 O1 . . 111.1(3) ? C1 C8 C9 . . 129.4(3) ? O1 C8 C9 . . 118.8(3) ? C8 C9 C10 . . 113.5(3) ? C8 C9 C16 . . 107.9(3) ? C10 C9 C16 . . 111.0(3) ? C8 C9 H9 . . 108.1 ? C10 C9 H9 . . 108.1 ? C16 C9 H9 . . 108.1 ? C15 C10 C11 . . 118.5(4) ? C15 C10 C9 . . 120.1(4) ? C11 C10 C9 . . 121.4(4) ? C10 C11 C12 . . 120.5(4) ? C10 C11 H11 . . 119.7 ? C12 C11 H11 . . 119.7 ? C13 C12 C11 . . 119.9(4) ? C13 C12 H12 . . 120.1 ? C11 C12 H12 . . 120.1 ? C14 C13 C12 . . 120.6(4) ? C14 C13 H13 . . 119.7 ? C12 C13 H13 . . 119.7 ? C13 C14 C15 . . 119.9(5) ? C13 C14 H14 . . 120.1 ? C15 C14 H14 . . 120.1 ? C10 C15 C14 . . 120.6(4) ? C10 C15 H15 . . 119.7 ? C14 C15 H15 . . 119.7 ? C17 C16 C19 . . 110.2(3) ? C17 C16 C9 . . 111.4(3) ? C19 C16 C9 . . 112.7(3) ? C17 C16 H16 . . 107.4 ? C19 C16 H16 . . 107.4 ? C9 C16 H16 . . 107.4 ? C18B C17 C16 . . 129.7(7) ? C18A C17 C16 . . 130.0(13) ? C18A C17 H17A . . 115.0 ? C16 C17 H17A . . 115.0 ? C18B C17 H17B . . 115.2 ? C16 C17 H17B . . 115.2 ? C17 C18A H18A . . 120.0 ? C17 C18A H18B . . 120.0 ? H18A C18A H18B . . 120.0 ? C17 C18B H18C . . 120.0 ? C17 C18B H18D . . 120.0 ? H18C C18B H18D . . 120.0 ? O2 C19 N1 . . 106.5(3) ? O2 C19 C16 . . 107.9(3) ? N1 C19 C16 . . 114.0(3) ? O2 C19 H19 . . 109.4 ? N1 C19 H19 . . 109.4 ? C16 C19 H19 . . 109.4 ? O3 C20 O2 . . 124.0(4) ? O3 C20 C21 . . 125.7(4) ? O2 C20 C21 . . 110.3(4) ? C20 C21 H21A . . 109.5 ? C20 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C20 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? C27 C22 C23 . . 120.6(4) ? C27 C22 S1 . . 120.0(3) ? C23 C22 S1 . . 119.4(3) ? C22 C23 C24 . . 119.0(5) ? C22 C23 H23 . . 120.5 ? C24 C23 H23 . . 120.5 ? C23 C24 C25 . . 121.2(5) ? C23 C24 H24 . . 119.4 ? C25 C24 H24 . . 119.4 ? C26 C25 C24 . . 117.9(4) ? C26 C25 C28 . . 122.6(6) ? C24 C25 C28 . . 119.6(6) ? C25 C26 C27 . . 122.2(5) ? C25 C26 H26 . . 118.9 ? C27 C26 H26 . . 118.9 ? C26 C27 C22 . . 119.1(4) ? C26 C27 H27 . . 120.4 ? C22 C27 H27 . . 120.4 ? C25 C28 H28A . . 109.5 ? C25 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C25 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C1 N1 C19 . . 112.7(3) ? C1 N1 S1 . . 118.9(2) ? C19 N1 S1 . . 117.9(2) ? C8 O1 C7 . . 105.6(3) ? C20 O2 C19 . . 116.9(3) ? O4 S1 O5 . . 120.81(19) ? O4 S1 N1 . . 105.20(17) ? O5 S1 N1 . . 106.01(17) ? O4 S1 C22 . . 108.32(18) ? O5 S1 C22 . . 108.71(19) ? N1 S1 C22 . . 106.99(16) ? C30 C29 H29A . . 109.5 ? C30 C29 H29B . . 109.5 ? H29A C29 H29B . . 109.5 ? C30 C29 H29C . . 109.5 ? H29A C29 H29C . . 109.5 ? H29B C29 H29C . . 109.5 ? O7 C30 O6 . . 122.7(8) ? O7 C30 C29 . . 113.6(7) ? O6 C30 C29 . . 123.7(8) ? C32 C31 O7 . . 111.4(6) ? C32 C31 H31A . . 109.4 ? O7 C31 H31A . . 109.4 ? C32 C31 H31B . . 109.4 ? O7 C31 H31B . . 109.4 ? H31A C31 H31B . . 108.0 ? C31 C32 H32A . . 109.5 ? C31 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? C31 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? C30 O7 C31 . . 119.9(6) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C8 . 1.342(5) ? C1 N1 . 1.429(5) ? C1 C2 . 1.441(5) ? C2 C7 . 1.383(6) ? C2 C3 . 1.398(6) ? C3 C4 . 1.384(7) ? C3 H3 . 0.94 ? C4 C5 . 1.397(8) ? C4 H4 . 0.94 ? C5 C6 . 1.370(7) ? C5 H5 . 0.94 ? C6 C7 . 1.384(6) ? C6 H6 . 0.94 ? C7 O1 . 1.376(5) ? C8 O1 . 1.368(4) ? C8 C9 . 1.478(5) ? C9 C10 . 1.516(5) ? C9 C16 . 1.560(5) ? C9 H9 . 0.99 ? C10 C15 . 1.378(6) ? C10 C11 . 1.379(6) ? C11 C12 . 1.394(7) ? C11 H11 . 0.94 ? C12 C13 . 1.364(8) ? C12 H12 . 0.94 ? C13 C14 . 1.352(7) ? C13 H13 . 0.94 ? C14 C15 . 1.400(6) ? C14 H14 . 0.94 ? C15 H15 . 0.94 ? C16 C17 . 1.505(6) ? C16 C19 . 1.526(5) ? C16 H16 . 0.99 ? C17 C18B . 1.226(9) ? C17 C18A . 1.24(2) ? C17 H17A . 0.94 ? C17 H17B . 0.94 ? C18A H18A . 0.94 ? C18A H18B . 0.94 ? C18B H18C . 0.94 ? C18B H18D . 0.94 ? C19 O2 . 1.437(5) ? C19 N1 . 1.464(5) ? C19 H19 . 0.99 ? C20 O3 . 1.179(6) ? C20 O2 . 1.358(5) ? C20 C21 . 1.499(7) ? C21 H21A . 0.97 ? C21 H21B . 0.97 ? C21 H21C . 0.97 ? C22 C27 . 1.382(6) ? C22 C23 . 1.384(6) ? C22 S1 . 1.750(4) ? C23 C24 . 1.388(7) ? C23 H23 . 0.94 ? C24 C25 . 1.397(8) ? C24 H24 . 0.94 ? C25 C26 . 1.372(7) ? C25 C28 . 1.488(7) ? C26 C27 . 1.379(6) ? C26 H26 . 0.94 ? C27 H27 . 0.94 ? C28 H28A . 0.97 ? C28 H28B . 0.97 ? C28 H28C . 0.97 ? N1 S1 . 1.668(3) ? O4 S1 . 1.421(3) ? O5 S1 . 1.425(3) ? C29 C30 . 1.430(11) ? C29 H29A . 0.97 ? C29 H29B . 0.97 ? C29 H29C . 0.97 ? C30 O7 . 1.234(9) ? C30 O6 . 1.235(10) ? C31 C32 . 1.425(12) ? C31 O7 . 1.508(9) ? C31 H31A . 0.98 ? C31 H31B . 0.98 ? C32 H32A . 0.97 ? C32 H32B . 0.97 ? C32 H32C . 0.97 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C9 H9 O4 3_646 0.99 2.61 3.454(5) 142.8 ? C19 H19 O5 . 0.99 2.41 2.907(5) 110.1 ? C21 H21A O6 3_646 0.97 2.50 3.349(8) 146.4 ? C32 H32A O6 . 0.97 2.61 3.110(11) 112.6 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C8 C1 C2 C7 . . . . 0.9(4) ? N1 C1 C2 C7 . . . . 170.5(4) ? C8 C1 C2 C3 . . . . -173.3(4) ? N1 C1 C2 C3 . . . . -3.7(7) ? C7 C2 C3 C4 . . . . 0.5(6) ? C1 C2 C3 C4 . . . . 174.0(4) ? C2 C3 C4 C5 . . . . -0.1(7) ? C3 C4 C5 C6 . . . . 0.1(8) ? C4 C5 C6 C7 . . . . -0.5(7) ? C3 C2 C7 O1 . . . . 175.1(3) ? C1 C2 C7 O1 . . . . -0.4(4) ? C3 C2 C7 C6 . . . . -1.0(6) ? C1 C2 C7 C6 . . . . -176.4(4) ? C5 C6 C7 O1 . . . . -174.6(4) ? C5 C6 C7 C2 . . . . 1.0(7) ? N1 C1 C8 O1 . . . . -171.9(3) ? C2 C1 C8 O1 . . . . -1.1(4) ? N1 C1 C8 C9 . . . . -1.0(6) ? C2 C1 C8 C9 . . . . 169.8(4) ? C1 C8 C9 C10 . . . . 131.7(4) ? O1 C8 C9 C10 . . . . -58.0(5) ? C1 C8 C9 C16 . . . . 8.2(5) ? O1 C8 C9 C16 . . . . 178.5(3) ? C8 C9 C10 C15 . . . . -51.1(5) ? C16 C9 C10 C15 . . . . 70.6(5) ? C8 C9 C10 C11 . . . . 128.6(4) ? C16 C9 C10 C11 . . . . -109.6(4) ? C15 C10 C11 C12 . . . . 0.6(7) ? C9 C10 C11 C12 . . . . -179.2(4) ? C10 C11 C12 C13 . . . . -1.3(8) ? C11 C12 C13 C14 . . . . 1.7(8) ? C12 C13 C14 C15 . . . . -1.3(8) ? C11 C10 C15 C14 . . . . -0.2(7) ? C9 C10 C15 C14 . . . . 179.5(4) ? C13 C14 C15 C10 . . . . 0.6(7) ? C8 C9 C16 C17 . . . . -157.8(4) ? C10 C9 C16 C17 . . . . 77.2(5) ? C8 C9 C16 C19 . . . . -33.4(4) ? C10 C9 C16 C19 . . . . -158.4(3) ? C19 C16 C17 C18B . . . . 103.8(8) ? C9 C16 C17 C18B . . . . -130.3(7) ? C19 C16 C17 C18A . . . . 36.(2) ? C9 C16 C17 C18A . . . . 162.(2) ? C17 C16 C19 O2 . . . . 62.3(4) ? C9 C16 C19 O2 . . . . -62.8(4) ? C17 C16 C19 N1 . . . . -179.5(4) ? C9 C16 C19 N1 . . . . 55.4(4) ? C27 C22 C23 C24 . . . . 0.3(7) ? S1 C22 C23 C24 . . . . -177.2(4) ? C22 C23 C24 C25 . . . . 0.9(7) ? C23 C24 C25 C26 . . . . -1.9(8) ? C23 C24 C25 C28 . . . . 179.3(5) ? C24 C25 C26 C27 . . . . 1.9(7) ? C28 C25 C26 C27 . . . . -179.4(5) ? C25 C26 C27 C22 . . . . -0.7(6) ? C23 C22 C27 C26 . . . . -0.4(6) ? S1 C22 C27 C26 . . . . 177.1(3) ? C8 C1 N1 C19 . . . . 20.1(5) ? C2 C1 N1 C19 . . . . -148.4(4) ? C8 C1 N1 S1 . . . . -124.0(3) ? C2 C1 N1 S1 . . . . 67.5(5) ? O2 C19 N1 C1 . . . . 72.0(4) ? C16 C19 N1 C1 . . . . -46.9(4) ? O2 C19 N1 S1 . . . . -143.5(2) ? C16 C19 N1 S1 . . . . 97.6(3) ? C1 C8 O1 C7 . . . . 0.9(4) ? C9 C8 O1 C7 . . . . -171.1(3) ? C2 C7 O1 C8 . . . . -0.3(4) ? C6 C7 O1 C8 . . . . 175.8(4) ? O3 C20 O2 C19 . . . . -0.4(6) ? C21 C20 O2 C19 . . . . -180.0(4) ? N1 C19 O2 C20 . . . . 102.8(4) ? C16 C19 O2 C20 . . . . -134.3(3) ? C1 N1 S1 O4 . . . . -46.7(3) ? C19 N1 S1 O4 . . . . 171.0(3) ? C1 N1 S1 O5 . . . . -175.8(3) ? C19 N1 S1 O5 . . . . 41.9(3) ? C1 N1 S1 C22 . . . . 68.3(3) ? C19 N1 S1 C22 . . . . -74.0(3) ? C27 C22 S1 O4 . . . . 27.8(4) ? C23 C22 S1 O4 . . . . -154.6(3) ? C27 C22 S1 O5 . . . . 160.8(3) ? C23 C22 S1 O5 . . . . -21.6(4) ? C27 C22 S1 N1 . . . . -85.2(3) ? C23 C22 S1 N1 . . . . 92.4(4) ? O6 C30 O7 C31 . . . . 0.3(11) ? C29 C30 O7 C31 . . . . -178.1(7) ? C32 C31 O7 C30 . . . . -79.3(9) ?