#------------------------------------------------------------------------------ #$Date: 2021-07-21 08:24:12 +0300 (Wed, 21 Jul 2021) $ #$Revision: 267668 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243875.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2243875 loop_ _publ_author_name 'Rousselin, Yoann' 'Yolka, Sylvie' 'Clavel, Alexandre' _publ_section_title ; Crystal structures of two polymorphs of tixocortol pivalate ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 809 _journal_page_last 813 _journal_paper_doi 10.1107/S2056989021007167 _journal_volume 77 _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_iupac 'C26 H38 O5 S' _chemical_formula_moiety 'C26 H38 O5 S' _chemical_formula_sum 'C26 H38 O5 S' _chemical_formula_weight 462.62 _chemical_name_systematic ;(S)-{2-[(8S,9S,10R,11S,13S,14S,17R)-11,17-Dihydroxy-10,13-dimethyl-3-oxo-2,6,7,8,9,11,12,14,15,16-decahydro-1H-cyclopenta[a]phenanthren-17-yl]-2-oxoethyl} 2,2-dimethylpropanethioate ; _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 _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.0146(2) _cell_length_b 19.2817(7) _cell_length_c 20.9887(7) _cell_measurement_reflns_used 6178 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 66.51 _cell_measurement_theta_min 3.11 _cell_volume 2434.10(14) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; ShelXL (Sheldrick, 2015b) ; _computing_structure_solution ; ShelXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.00(10) _diffrn_detector CMOS _diffrn_detector_area_resol_mean '1024 x 1024' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'QUAZAR MX multilayer optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_unetI/netI 0.0541 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 30900 _diffrn_reflns_theta_full 66.740 _diffrn_reflns_theta_max 66.740 _diffrn_reflns_theta_min 3.112 _diffrn_source 'sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_T_max 0.8622 _exptl_absorpt_correction_T_min 0.7073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.262 _exptl_crystal_description plate _exptl_crystal_F_000 1000 _exptl_crystal_size_max 0.184 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.264 _refine_diff_density_min -0.389 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.11(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4303 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0551 _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^)+(0.0520P)^2^+1.3292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1256 _refine_ls_wR_factor_ref 0.1303 _reflns_number_gt 3803 _reflns_number_total 4303 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL SY20C174 in P2(1)2(1)2(1) SY20C174.res created by SHELXL-2018/3 at 13:46:17 on 11-Sep-2020 CELL 1.54178 6.0146 19.2817 20.9887 90 90 90 ZERR 4 0.0002 0.0007 0.0007 0 0 0 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 O S UNIT 104 152 20 4 EQIV $1 0.5-X,1-Y,0.5+Z SADI 0.001 C6 S1 C6 S1A L.S. 10 PLAN 10 SIZE 0.05 0.063 0.184 TEMP -173.15(10) HTAB O3 O5_$1 BOND $H HTAB CONF list 4 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.052000 1.329200 BASF 0.11485 FVAR 0.52789 0.76980 O2 3 0.589869 0.436049 0.723791 11.00000 0.05727 0.06557 = 0.03977 -0.01335 -0.01475 -0.00322 O3 3 0.215562 0.506166 0.613391 11.00000 0.04348 0.03030 = 0.04336 -0.01069 -0.00084 0.00779 AFIX 147 H3 2 0.209393 0.545661 0.630189 11.00000 -1.50000 AFIX 0 O4 3 0.452314 0.283627 0.491530 11.00000 0.05644 0.02082 = 0.03284 0.00141 0.00559 -0.00096 AFIX 147 H4 2 0.369010 0.253012 0.507049 11.00000 -1.50000 AFIX 0 O5 3 0.295541 0.366007 0.176775 11.00000 0.07655 0.03983 = 0.02974 0.00319 -0.00419 0.01353 C19 1 0.582430 0.409947 0.320693 11.00000 0.03371 0.03099 = 0.03479 0.00745 0.00979 0.00977 C23 1 0.507461 0.412550 0.260549 11.00000 0.04854 0.03026 = 0.03637 0.00788 0.01115 0.00921 AFIX 43 H23 2 0.550048 0.451088 0.235126 11.00000 -1.20000 AFIX 0 C10 1 0.550777 0.474391 0.517942 11.00000 0.02889 0.02529 = 0.04315 -0.00171 -0.00523 -0.00005 AFIX 13 H10 2 0.415291 0.501122 0.505311 11.00000 -1.20000 AFIX 0 C26 1 0.297386 0.318239 0.341593 11.00000 0.03324 0.02951 = 0.03094 0.00255 0.00269 -0.00311 AFIX 23 H26A 2 0.270014 0.275824 0.366990 11.00000 -1.20000 H26B 2 0.167597 0.349225 0.347184 11.00000 -1.20000 AFIX 0 C21 1 0.700977 0.491480 0.408424 11.00000 0.03087 0.02630 = 0.04671 0.00374 0.00023 -0.00325 AFIX 23 H21A 2 0.832545 0.517167 0.424124 11.00000 -1.20000 H21B 2 0.578497 0.525229 0.402795 11.00000 -1.20000 AFIX 0 C18 1 0.505211 0.354809 0.367724 11.00000 0.03177 0.02563 = 0.02904 0.00553 0.00169 0.00059 C24 1 0.366372 0.360653 0.231936 11.00000 0.05347 0.03775 = 0.03055 0.00349 0.00678 0.01743 C15 1 0.326924 0.346022 0.481328 11.00000 0.03599 0.02238 = 0.03043 -0.00132 -0.00034 -0.00324 AFIX 13 H15 2 0.180184 0.332125 0.462922 11.00000 -1.20000 AFIX 0 C8 1 0.426954 0.475982 0.625835 11.00000 0.04007 0.03176 = 0.04401 -0.00905 -0.00495 0.00470 C17 1 0.632671 0.438001 0.458176 11.00000 0.02573 0.02375 = 0.03821 0.00198 -0.00284 0.00221 AFIX 13 H17 2 0.763081 0.408045 0.468950 11.00000 -1.20000 AFIX 0 C9 1 0.477217 0.423688 0.570669 11.00000 0.03278 0.02717 = 0.03675 -0.00330 -0.00200 0.00147 C22 1 0.697131 0.301916 0.374367 11.00000 0.04220 0.02840 = 0.03303 0.00180 0.00376 0.00311 AFIX 137 H22A 2 0.751711 0.289182 0.331957 11.00000 -1.50000 H22B 2 0.642942 0.260357 0.396306 11.00000 -1.50000 H22C 2 0.818350 0.322694 0.399048 11.00000 -1.50000 AFIX 0 C11 1 0.705202 0.525664 0.551158 11.00000 0.03569 0.03019 = 0.05025 -0.00568 -0.00748 -0.00194 AFIX 23 H11A 2 0.698529 0.571722 0.530401 11.00000 -1.20000 H11B 2 0.860739 0.508887 0.550330 11.00000 -1.20000 AFIX 0 C20 1 0.756419 0.458907 0.343805 11.00000 0.03589 0.03106 = 0.04656 0.00950 0.00797 -0.00035 AFIX 23 H20A 2 0.775716 0.496321 0.311979 11.00000 -1.20000 H20B 2 0.899444 0.433782 0.347301 11.00000 -1.20000 AFIX 0 C12 1 0.617372 0.529542 0.620181 11.00000 0.04599 0.03691 = 0.05138 -0.01491 -0.00667 -0.00109 AFIX 23 H12A 2 0.561469 0.576745 0.629549 11.00000 -1.20000 H12B 2 0.737654 0.518446 0.650724 11.00000 -1.20000 AFIX 0 C6 1 0.207597 0.408797 0.713805 11.00000 0.05805 0.04144 = 0.03271 -0.00037 -0.00188 0.01168 PART 1 AFIX 23 H6AA 2 0.196918 0.361138 0.696528 21.00000 -1.20000 H6AB 2 0.082226 0.435978 0.696182 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H6BC 2 0.120508 0.394023 0.676151 -21.00000 -1.20000 H6BD 2 0.119404 0.443918 0.737153 -21.00000 -1.20000 AFIX 0 PART 0 C13 1 0.666869 0.375226 0.591806 11.00000 0.04337 0.03388 = 0.03697 -0.00555 -0.00598 0.00545 AFIX 137 H13A 2 0.721108 0.348936 0.554993 11.00000 -1.50000 H13B 2 0.611557 0.343021 0.624265 11.00000 -1.50000 H13C 2 0.788640 0.402879 0.609613 11.00000 -1.50000 AFIX 0 C25 1 0.315112 0.298272 0.271614 11.00000 0.04356 0.03618 = 0.03224 0.00023 -0.00202 0.00443 AFIX 23 H25A 2 0.433983 0.263261 0.266140 11.00000 -1.20000 H25B 2 0.173190 0.277449 0.257299 11.00000 -1.20000 AFIX 0 C14 1 0.279597 0.383682 0.544778 11.00000 0.03192 0.02542 = 0.03363 0.00075 0.00406 -0.00184 AFIX 23 H14A 2 0.154299 0.416247 0.538403 11.00000 -1.20000 H14B 2 0.232769 0.349021 0.576884 11.00000 -1.20000 AFIX 0 C7 1 0.424197 0.440975 0.691915 11.00000 0.05235 0.03754 = 0.03656 -0.01616 -0.00386 0.00393 C16 1 0.443907 0.392821 0.431589 11.00000 0.02587 0.02230 = 0.03268 0.00485 -0.00078 0.00156 AFIX 13 H16 2 0.326901 0.426958 0.418849 11.00000 -1.20000 AFIX 0 PART 1 S1 4 0.181474 0.405370 0.799353 21.00000 0.06276 0.04130 = 0.03087 -0.00082 0.00248 0.02059 O1 3 0.348334 0.285009 0.768362 21.00000 0.05190 0.04152 = 0.04177 -0.01288 -0.01472 0.00672 C1 1 0.352128 0.302827 0.881318 21.00000 0.04068 0.03138 = 0.03615 -0.00836 -0.00094 0.00845 C2 1 0.609002 0.307615 0.887798 21.00000 0.03300 0.04436 = 0.03932 -0.00748 -0.00721 0.00509 AFIX 137 H2A 2 0.652836 0.294448 0.931111 21.00000 -1.50000 H2B 2 0.657117 0.355274 0.879249 21.00000 -1.50000 H2C 2 0.679074 0.276143 0.857122 21.00000 -1.50000 AFIX 0 C4 1 0.272465 0.229112 0.892830 21.00000 0.07132 0.03691 = 0.06614 0.01177 -0.01272 0.00109 AFIX 137 H4A 2 0.339000 0.198135 0.861101 21.00000 -1.50000 H4B 2 0.110117 0.227401 0.889187 21.00000 -1.50000 H4C 2 0.316890 0.214251 0.935628 21.00000 -1.50000 AFIX 0 C3 1 0.243824 0.352097 0.930239 21.00000 0.04107 0.04344 = 0.03683 -0.00149 -0.00064 0.00634 AFIX 137 H3A 2 0.278848 0.336261 0.973456 21.00000 -1.50000 H3B 2 0.082257 0.352166 0.924197 21.00000 -1.50000 H3C 2 0.301585 0.399154 0.924132 21.00000 -1.50000 AFIX 0 C5 1 0.302239 0.322971 0.811884 21.00000 0.03213 0.03017 = 0.03726 -0.00386 -0.00013 0.00060 SAME 0.02 0.04 S1 > C5 PART 0 PART 2 S1A 4 0.255279 0.334878 0.764901 -21.00000 0.05453 O1A 3 0.296869 0.431393 0.849585 -21.00000 0.04242 C1A 1 0.355387 0.318653 0.897155 -21.00000 0.02306 C2A 1 0.614636 0.309096 0.898809 -21.00000 0.05956 AFIX 137 H2AA 2 0.683993 0.351239 0.915726 -21.00000 -1.50000 H2AB 2 0.669427 0.300462 0.855557 -21.00000 -1.50000 H2AC 2 0.652259 0.269623 0.926175 -21.00000 -1.50000 AFIX 0 C3A 1 0.282958 0.346311 0.960903 -21.00000 0.05589 AFIX 137 H3AA 2 0.340463 0.316272 0.994771 -21.00000 -1.50000 H3AB 2 0.120195 0.347280 0.962866 -21.00000 -1.50000 H3AC 2 0.341046 0.393392 0.966587 -21.00000 -1.50000 AFIX 0 C4A 1 0.260359 0.245521 0.882027 -21.00000 0.03836 AFIX 137 H4AA 2 0.330574 0.227462 0.843296 -21.00000 -1.50000 H4AB 2 0.099349 0.248796 0.875531 -21.00000 -1.50000 H4AC 2 0.291241 0.214194 0.917714 -21.00000 -1.50000 AFIX 0 C5A 1 0.310301 0.369500 0.841243 -21.00000 0.04080 HKLF 4 REM SY20C174 in P2(1)2(1)2(1) REM wR2 = 0.1303, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0551 for 3803 Fo > 4sig(Fo) and 0.0639 for all 4303 data REM 329 parameters refined using 16 restraints END WGHT 0.0520 1.3291 REM Instructions for potential hydrogen bonds HTAB O3 O5_$1 EQIV $2 x-1/2, -y+1/2, -z+1 HTAB O4 O4_$2 HTAB C12 O5_$1 EQIV $3 x+1/2, -y+1/2, -z+1 HTAB C25 S1A_$3 HTAB C25 O1_$2 REM Highest difference peak 0.264, deepest hole -0.389, 1-sigma level 0.050 Q1 1 0.2217 0.3184 0.7789 11.00000 0.05 0.26 Q2 1 0.2099 0.4360 0.7647 11.00000 0.05 0.18 Q3 1 0.1851 0.4233 0.7246 11.00000 0.05 0.18 Q4 1 0.1285 0.3682 0.1658 11.00000 0.05 0.17 Q5 1 0.0934 0.3591 1.0546 11.00000 0.05 0.16 Q6 1 1.1005 0.4614 0.3467 11.00000 0.05 0.16 Q7 1 0.1735 0.4400 0.8332 11.00000 0.05 0.15 Q8 1 0.6681 0.4130 0.7744 11.00000 0.05 0.15 Q9 1 0.4000 0.2203 0.2037 11.00000 0.05 0.15 Q10 1 0.4429 0.3771 0.4665 11.00000 0.05 0.15 REM The information below was added by Olex2. REM REM R1 = 0.0551 for 3803 Fo > 4sig(Fo) and 0.0639 for all 31030 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.26, deepest hole -0.39 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0639 REM R1_gt = 0.0551 REM wR_ref = 0.1303 REM GOOF = 1.065 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 31030 REM Reflections_gt = 3803 REM Parameters = n/a REM Hole = -0.39 REM Peak = 0.26 REM Flack = n/a ; _cod_data_source_file dj2019sup1.cif _cod_data_source_block SY20C174 _cod_database_code 2243875 _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 0.776 _shelx_estimated_absorpt_t_max 0.931 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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O2 0.5899(6) 0.4360(2) 0.72379(16) 0.0542(10) Uani d 1 . . O O3 0.2156(5) 0.50617(16) 0.61339(15) 0.0390(7) Uani d 1 . . H H3 0.209393 0.545661 0.630189 0.059 Uiso calc 1 . . O O4 0.4523(5) 0.28363(14) 0.49153(14) 0.0367(7) Uani d 1 . . H H4 0.369010 0.253012 0.507049 0.055 Uiso calc 1 . . O O5 0.2955(7) 0.36601(17) 0.17678(14) 0.0487(9) Uani d 1 . . C C19 0.5824(7) 0.4099(2) 0.3207(2) 0.0332(9) Uani d 1 . . C C23 0.5075(8) 0.4126(2) 0.2605(2) 0.0384(10) Uani d 1 . . H H23 0.550048 0.451088 0.235126 0.046 Uiso calc 1 . . C C10 0.5508(7) 0.4744(2) 0.5179(2) 0.0324(9) Uani d 1 . . H H10 0.415291 0.501122 0.505311 0.039 Uiso calc 1 . . C C26 0.2974(7) 0.3182(2) 0.34159(18) 0.0312(9) Uani d 1 . . H H26A 0.270014 0.275824 0.366990 0.037 Uiso calc 1 . . H H26B 0.167597 0.349225 0.347184 0.037 Uiso calc 1 . . C C21 0.7010(7) 0.4915(2) 0.4084(2) 0.0346(9) Uani d 1 . . H H21A 0.832545 0.517167 0.424124 0.042 Uiso calc 1 . . H H21B 0.578497 0.525229 0.402795 0.042 Uiso calc 1 . . C C18 0.5052(7) 0.3548(2) 0.36772(19) 0.0288(9) Uani d 1 . . C C24 0.3664(8) 0.3607(2) 0.2319(2) 0.0406(11) Uani d 1 . . C C15 0.3269(7) 0.34602(19) 0.48133(19) 0.0296(9) Uani d 1 . . H H15 0.180184 0.332125 0.462922 0.036 Uiso calc 1 . . C C8 0.4270(8) 0.4760(2) 0.6258(2) 0.0386(10) Uani d 1 . . C C17 0.6327(7) 0.4380(2) 0.4582(2) 0.0292(9) Uani d 1 . . H H17 0.763081 0.408045 0.468950 0.035 Uiso calc 1 . . C C9 0.4772(7) 0.4237(2) 0.5707(2) 0.0322(10) Uani d 1 . . C C22 0.6971(8) 0.3019(2) 0.3744(2) 0.0345(9) Uani d 1 . . H H22A 0.751711 0.289182 0.331957 0.052 Uiso calc 1 . . H H22B 0.642942 0.260357 0.396306 0.052 Uiso calc 1 . . H H22C 0.818350 0.322694 0.399048 0.052 Uiso calc 1 . . C C11 0.7052(8) 0.5257(2) 0.5512(2) 0.0387(10) Uani d 1 . . H H11A 0.698529 0.571722 0.530401 0.046 Uiso calc 1 . . H H11B 0.860739 0.508887 0.550330 0.046 Uiso calc 1 . . C C20 0.7564(7) 0.4589(2) 0.3438(2) 0.0378(11) Uani d 1 . . H H20A 0.775716 0.496321 0.311979 0.045 Uiso calc 1 . . H H20B 0.899444 0.433782 0.347301 0.045 Uiso calc 1 . . C C12 0.6174(8) 0.5295(3) 0.6202(2) 0.0448(12) Uani d 1 . . H H12A 0.561469 0.576745 0.629549 0.054 Uiso calc 1 . . H H12B 0.737654 0.518446 0.650724 0.054 Uiso calc 1 . . C C6 0.2076(9) 0.4088(2) 0.7138(2) 0.0441(11) Uani d 1 . . H H6AA 0.196918 0.361138 0.696528 0.053 Uiso calc 0.770(4) A 1 H H6AB 0.082226 0.435978 0.696182 0.053 Uiso calc 0.770(4) A 1 H H6BC 0.120508 0.394023 0.676151 0.053 Uiso calc 0.230(4) A 2 H H6BD 0.119404 0.443918 0.737153 0.053 Uiso calc 0.230(4) A 2 C C13 0.6669(8) 0.3752(2) 0.5918(2) 0.0381(10) Uani d 1 . . H H13A 0.721108 0.348936 0.554993 0.057 Uiso calc 1 . . H H13B 0.611557 0.343021 0.624265 0.057 Uiso calc 1 . . H H13C 0.788640 0.402879 0.609613 0.057 Uiso calc 1 . . C C25 0.3151(8) 0.2983(2) 0.27161(19) 0.0373(10) Uani d 1 . . H H25A 0.433983 0.263261 0.266140 0.045 Uiso calc 1 . . H H25B 0.173190 0.277449 0.257299 0.045 Uiso calc 1 . . C C14 0.2796(7) 0.3837(2) 0.54478(19) 0.0303(9) Uani d 1 . . H H14A 0.154299 0.416247 0.538403 0.036 Uiso calc 1 . . H H14B 0.232769 0.349021 0.576884 0.036 Uiso calc 1 . . C C7 0.4242(9) 0.4410(2) 0.6919(2) 0.0421(11) Uani d 1 . . C C16 0.4439(7) 0.39282(19) 0.43159(19) 0.0270(9) Uani d 1 . . H H16 0.326901 0.426958 0.418849 0.032 Uiso calc 1 . . S S1 0.1815(3) 0.40537(8) 0.79935(7) 0.0450(5) Uani d 0.770(4) A 1 O O1 0.3483(7) 0.2850(2) 0.76836(19) 0.0451(11) Uani d 0.770(4) A 1 C C1 0.3521(12) 0.3028(4) 0.8813(3) 0.0361(18) Uani d 0.770(4) A 1 C C2 0.6090(12) 0.3076(8) 0.8878(8) 0.039(3) Uani d 0.770(4) A 1 H H2A 0.652836 0.294448 0.931111 0.058 Uiso calc 0.770(4) A 1 H H2B 0.657117 0.355274 0.879249 0.058 Uiso calc 0.770(4) A 1 H H2C 0.679074 0.276143 0.857122 0.058 Uiso calc 0.770(4) A 1 C C4 0.272(2) 0.2291(5) 0.8928(5) 0.058(3) Uani d 0.770(4) A 1 H H4A 0.339000 0.198135 0.861101 0.087 Uiso calc 0.770(4) A 1 H H4B 0.110117 0.227401 0.889187 0.087 Uiso calc 0.770(4) A 1 H H4C 0.316890 0.214251 0.935628 0.087 Uiso calc 0.770(4) A 1 C C3 0.2438(11) 0.3521(3) 0.9302(3) 0.0404(15) Uani d 0.770(4) A 1 H H3A 0.278848 0.336261 0.973456 0.061 Uiso calc 0.770(4) A 1 H H3B 0.082257 0.352166 0.924197 0.061 Uiso calc 0.770(4) A 1 H H3C 0.301585 0.399154 0.924132 0.061 Uiso calc 0.770(4) A 1 C C5 0.3022(10) 0.3230(3) 0.8119(3) 0.0332(12) Uani d 0.770(4) A 1 S S1A 0.2553(10) 0.3349(3) 0.7649(3) 0.055(2) Uiso d 0.230(4) A 2 O O1A 0.297(2) 0.4314(7) 0.8496(6) 0.042(4) Uiso d 0.230(4) A 2 C C1A 0.355(4) 0.3187(10) 0.8972(9) 0.023(7) Uiso d 0.230(4) A 2 C C2A 0.615(5) 0.309(3) 0.899(3) 0.06(2) Uiso d 0.230(4) A 2 H H2AA 0.683993 0.351239 0.915726 0.089 Uiso calc 0.230(4) A 2 H H2AB 0.669427 0.300462 0.855557 0.089 Uiso calc 0.230(4) A 2 H H2AC 0.652259 0.269623 0.926175 0.089 Uiso calc 0.230(4) A 2 C C3A 0.283(5) 0.3463(15) 0.9609(11) 0.056(8) Uiso d 0.230(4) A 2 H H3AA 0.340463 0.316272 0.994771 0.084 Uiso calc 0.230(4) A 2 H H3AB 0.120195 0.347280 0.962866 0.084 Uiso calc 0.230(4) A 2 H H3AC 0.341046 0.393392 0.966587 0.084 Uiso calc 0.230(4) A 2 C C4A 0.260(6) 0.2455(13) 0.8820(15) 0.038(8) Uiso d 0.230(4) A 2 H H4AA 0.330574 0.227462 0.843296 0.058 Uiso calc 0.230(4) A 2 H H4AB 0.099349 0.248796 0.875531 0.058 Uiso calc 0.230(4) A 2 H H4AC 0.291241 0.214194 0.917714 0.058 Uiso calc 0.230(4) A 2 C C5A 0.310(3) 0.3695(9) 0.8412(8) 0.041(5) Uiso d 0.230(4) A 2 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 O2 0.057(2) 0.066(2) 0.0398(19) -0.0032(19) -0.0148(17) -0.0134(17) O3 0.0435(18) 0.0303(16) 0.0434(18) 0.0078(14) -0.0008(14) -0.0107(13) O4 0.056(2) 0.0208(14) 0.0328(16) -0.0010(14) 0.0056(15) 0.0014(12) O5 0.077(2) 0.0398(18) 0.0297(17) 0.0135(18) -0.0042(17) 0.0032(13) C19 0.034(2) 0.031(2) 0.035(2) 0.0098(18) 0.0098(18) 0.0075(18) C23 0.049(3) 0.030(2) 0.036(2) 0.009(2) 0.011(2) 0.008(2) C10 0.029(2) 0.025(2) 0.043(2) 0.0000(17) -0.0052(19) -0.0017(19) C26 0.033(2) 0.030(2) 0.031(2) -0.0031(18) 0.0027(19) 0.0025(17) C21 0.031(2) 0.026(2) 0.047(3) -0.0033(18) 0.000(2) 0.0037(18) C18 0.032(2) 0.026(2) 0.029(2) 0.0006(17) 0.0017(17) 0.0055(17) C24 0.053(3) 0.038(2) 0.031(2) 0.017(2) 0.007(2) 0.0035(19) C15 0.036(2) 0.022(2) 0.030(2) -0.0032(18) -0.0003(18) -0.0013(16) C8 0.040(2) 0.032(2) 0.044(3) 0.005(2) -0.005(2) -0.009(2) C17 0.026(2) 0.0237(19) 0.038(2) 0.0022(16) -0.0028(17) 0.0020(17) C9 0.033(2) 0.027(2) 0.037(2) 0.0015(17) -0.0020(18) -0.0033(18) C22 0.042(2) 0.028(2) 0.033(2) 0.003(2) 0.004(2) 0.0018(17) C11 0.036(2) 0.030(2) 0.050(3) -0.0019(19) -0.007(2) -0.006(2) C20 0.036(2) 0.031(2) 0.047(3) -0.0004(18) 0.008(2) 0.010(2) C12 0.046(3) 0.037(2) 0.051(3) -0.001(2) -0.007(2) -0.015(2) C6 0.058(3) 0.041(3) 0.033(2) 0.012(2) -0.002(2) 0.000(2) C13 0.043(3) 0.034(2) 0.037(2) 0.005(2) -0.006(2) -0.0056(19) C25 0.044(2) 0.036(2) 0.032(2) 0.004(2) -0.002(2) 0.0002(18) C14 0.032(2) 0.025(2) 0.034(2) -0.0018(17) 0.0041(17) 0.0008(17) C7 0.052(3) 0.038(2) 0.037(3) 0.004(2) -0.004(2) -0.016(2) C16 0.026(2) 0.0223(19) 0.033(2) 0.0016(16) -0.0008(17) 0.0049(16) S1 0.0628(10) 0.0413(9) 0.0309(8) 0.0206(8) 0.0025(7) -0.0008(6) O1 0.052(3) 0.042(2) 0.042(2) 0.007(2) -0.015(2) -0.013(2) C1 0.041(4) 0.031(4) 0.036(4) 0.008(3) -0.001(3) -0.008(3) C2 0.033(5) 0.044(6) 0.039(5) 0.005(3) -0.007(3) -0.007(4) C4 0.071(6) 0.037(4) 0.066(6) 0.001(4) -0.013(5) 0.012(4) C3 0.041(4) 0.043(4) 0.037(4) 0.006(3) -0.001(3) -0.001(3) C5 0.032(3) 0.030(3) 0.037(3) 0.001(2) 0.000(2) -0.004(3) 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' 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' 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 O3 H3 . . 109.5 ? C15 O4 H4 . . 109.5 ? C23 C19 C18 . . 122.2(4) ? C23 C19 C20 . . 121.2(4) ? C20 C19 C18 . . 116.4(4) ? C19 C23 H23 . . 117.9 ? C19 C23 C24 . . 124.3(4) ? C24 C23 H23 . . 117.9 ? C17 C10 H10 . . 106.5 ? C17 C10 C9 . . 113.1(3) ? C17 C10 C11 . . 118.6(4) ? C9 C10 H10 . . 106.5 ? C11 C10 H10 . . 106.5 ? C11 C10 C9 . . 104.9(4) ? H26A C26 H26B . . 107.7 ? C18 C26 H26A . . 108.8 ? C18 C26 H26B . . 108.8 ? C25 C26 H26A . . 108.8 ? C25 C26 H26B . . 108.8 ? C25 C26 C18 . . 113.8(4) ? H21A C21 H21B . . 107.8 ? C17 C21 H21A . . 109.0 ? C17 C21 H21B . . 109.0 ? C17 C21 C20 . . 112.8(3) ? C20 C21 H21A . . 109.0 ? C20 C21 H21B . . 109.0 ? C19 C18 C26 . . 109.7(3) ? C19 C18 C22 . . 106.9(3) ? C19 C18 C16 . . 107.4(3) ? C26 C18 C22 . . 109.7(3) ? C26 C18 C16 . . 109.1(3) ? C22 C18 C16 . . 113.9(3) ? O5 C24 C23 . . 122.3(4) ? O5 C24 C25 . . 121.1(5) ? C23 C24 C25 . . 116.6(4) ? O4 C15 H15 . . 107.3 ? O4 C15 C14 . . 111.2(3) ? O4 C15 C16 . . 110.5(3) ? C14 C15 H15 . . 107.3 ? C14 C15 C16 . . 113.0(3) ? C16 C15 H15 . . 107.3 ? O3 C8 C9 . . 107.5(3) ? O3 C8 C12 . . 112.0(4) ? O3 C8 C7 . . 109.5(4) ? C12 C8 C9 . . 103.3(4) ? C7 C8 C9 . . 112.7(4) ? C7 C8 C12 . . 111.7(4) ? C10 C17 C21 . . 109.9(3) ? C10 C17 H17 . . 109.5 ? C10 C17 C16 . . 108.8(3) ? C21 C17 H17 . . 109.5 ? C21 C17 C16 . . 109.5(3) ? C16 C17 H17 . . 109.5 ? C10 C9 C8 . . 100.3(3) ? C13 C9 C10 . . 112.3(4) ? C13 C9 C8 . . 108.7(3) ? C14 C9 C10 . . 106.9(3) ? C14 C9 C8 . . 116.2(4) ? C14 C9 C13 . . 112.0(3) ? C18 C22 H22A . . 109.5 ? C18 C22 H22B . . 109.5 ? C18 C22 H22C . . 109.5 ? H22A C22 H22B . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? C10 C11 H11A . . 110.8 ? C10 C11 H11B . . 110.8 ? C10 C11 C12 . . 104.6(4) ? H11A C11 H11B . . 108.9 ? C12 C11 H11A . . 110.8 ? C12 C11 H11B . . 110.8 ? C19 C20 C21 . . 113.3(4) ? C19 C20 H20A . . 108.9 ? C19 C20 H20B . . 108.9 ? C21 C20 H20A . . 108.9 ? C21 C20 H20B . . 108.9 ? H20A C20 H20B . . 107.7 ? C8 C12 H12A . . 110.3 ? C8 C12 H12B . . 110.3 ? C11 C12 C8 . . 107.0(4) ? C11 C12 H12A . . 110.3 ? C11 C12 H12B . . 110.3 ? H12A C12 H12B . . 108.6 ? H6AA C6 H6AB . . 107.8 ? H6BC C6 H6BD . . 108.0 ? C7 C6 H6AA . . 109.0 ? C7 C6 H6AB . . 109.0 ? C7 C6 H6BC . . 109.3 ? C7 C6 H6BD . . 109.3 ? C7 C6 S1 . . 113.1(4) ? C7 C6 S1A . . 111.5(4) ? S1 C6 H6AA . . 109.0 ? S1 C6 H6AB . . 109.0 ? S1A C6 H6BC . . 109.3 ? S1A C6 H6BD . . 109.3 ? C9 C13 H13A . . 109.5 ? C9 C13 H13B . . 109.5 ? C9 C13 H13C . . 109.5 ? H13A C13 H13B . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? C26 C25 H25A . . 109.6 ? C26 C25 H25B . . 109.6 ? C24 C25 C26 . . 110.4(4) ? C24 C25 H25A . . 109.6 ? C24 C25 H25B . . 109.6 ? H25A C25 H25B . . 108.1 ? C15 C14 H14A . . 108.8 ? C15 C14 H14B . . 108.8 ? C9 C14 C15 . . 113.8(3) ? C9 C14 H14A . . 108.8 ? C9 C14 H14B . . 108.8 ? H14A C14 H14B . . 107.7 ? O2 C7 C8 . . 121.7(5) ? O2 C7 C6 . . 120.7(5) ? C6 C7 C8 . . 117.5(4) ? C18 C16 H16 . . 104.1 ? C15 C16 C18 . . 114.2(3) ? C15 C16 H16 . . 104.1 ? C17 C16 C18 . . 113.6(3) ? C17 C16 C15 . . 114.9(3) ? C17 C16 H16 . . 104.1 ? C5 S1 C6 . . 98.4(2) ? C4 C1 C2 . . 110.8(8) ? C4 C1 C3 . . 109.7(6) ? C4 C1 C5 . . 109.0(7) ? C3 C1 C2 . . 109.0(9) ? C5 C1 C2 . . 105.2(7) ? C5 C1 C3 . . 113.1(5) ? C1 C2 H2A . . 109.5 ? C1 C2 H2B . . 109.5 ? C1 C2 H2C . . 109.5 ? H2A C2 H2B . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C1 C4 H4A . . 109.5 ? C1 C4 H4B . . 109.5 ? C1 C4 H4C . . 109.5 ? H4A C4 H4B . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C1 C3 H3A . . 109.5 ? C1 C3 H3B . . 109.5 ? C1 C3 H3C . . 109.5 ? H3A C3 H3B . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? O1 C5 S1 . . 121.9(4) ? O1 C5 C1 . . 121.4(5) ? C1 C5 S1 . . 116.6(4) ? C5A S1A C6 . . 105.7(6) ? C3A C1A C2A . . 108(3) ? C3A C1A C4A . . 113.4(19) ? C3A C1A C5A . . 113.4(17) ? C4A C1A C2A . . 105(3) ? C5A C1A C2A . . 105(2) ? C5A C1A C4A . . 110.7(17) ? C1A C2A H2AA . . 109.5 ? C1A C2A H2AB . . 109.5 ? C1A C2A H2AC . . 109.5 ? H2AA C2A H2AB . . 109.5 ? H2AA C2A H2AC . . 109.5 ? H2AB C2A H2AC . . 109.5 ? C1A C3A H3AA . . 109.5 ? C1A C3A H3AB . . 109.5 ? C1A C3A H3AC . . 109.5 ? H3AA C3A H3AB . . 109.5 ? H3AA C3A H3AC . . 109.5 ? H3AB C3A H3AC . . 109.5 ? C1A C4A H4AA . . 109.5 ? C1A C4A H4AB . . 109.5 ? C1A C4A H4AC . . 109.5 ? H4AA C4A H4AB . . 109.5 ? H4AA C4A H4AC . . 109.5 ? H4AB C4A H4AC . . 109.5 ? O1A C5A S1A . . 119.5(13) ? O1A C5A C1A . . 121.7(15) ? C1A C5A S1A . . 118.6(12) ? 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 O2 C7 . 1.204(6) ? O3 H3 . 0.8400 ? O3 C8 . 1.422(6) ? O4 H4 . 0.8400 ? O4 C15 . 1.436(5) ? O5 C24 . 1.238(5) ? C19 C23 . 1.341(6) ? C19 C18 . 1.523(6) ? C19 C20 . 1.491(6) ? C23 H23 . 0.9500 ? C23 C24 . 1.443(7) ? C10 H10 . 1.0000 ? C10 C17 . 1.519(6) ? C10 C9 . 1.542(6) ? C10 C11 . 1.525(6) ? C26 H26A . 0.9900 ? C26 H26B . 0.9900 ? C26 C18 . 1.536(6) ? C26 C25 . 1.522(5) ? C21 H21A . 0.9900 ? C21 H21B . 0.9900 ? C21 C17 . 1.524(6) ? C21 C20 . 1.531(6) ? C18 C22 . 1.547(6) ? C18 C16 . 1.572(6) ? C24 C25 . 1.495(6) ? C15 H15 . 1.0000 ? C15 C14 . 1.543(6) ? C15 C16 . 1.549(5) ? C8 C9 . 1.565(6) ? C8 C12 . 1.547(7) ? C8 C7 . 1.543(7) ? C17 H17 . 1.0000 ? C17 C16 . 1.536(6) ? C9 C13 . 1.540(6) ? C9 C14 . 1.518(6) ? C22 H22A . 0.9800 ? C22 H22B . 0.9800 ? C22 H22C . 0.9800 ? C11 H11A . 0.9900 ? C11 H11B . 0.9900 ? C11 C12 . 1.544(7) ? C20 H20A . 0.9900 ? C20 H20B . 0.9900 ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C6 H6AA . 0.9900 ? C6 H6AB . 0.9900 ? C6 H6BC . 0.9900 ? C6 H6BD . 0.9900 ? C6 C7 . 1.514(7) ? C6 S1 . 1.804(4) ? C6 S1A . 1.807(5) ? C13 H13A . 0.9800 ? C13 H13B . 0.9800 ? C13 H13C . 0.9800 ? C25 H25A . 0.9900 ? C25 H25B . 0.9900 ? C14 H14A . 0.9900 ? C14 H14B . 0.9900 ? C16 H16 . 1.0000 ? S1 C5 . 1.767(6) ? O1 C5 . 1.203(6) ? C1 C2 . 1.554(9) ? C1 C4 . 1.519(11) ? C1 C3 . 1.543(9) ? C1 C5 . 1.538(9) ? C2 H2A . 0.9800 ? C2 H2B . 0.9800 ? C2 H2C . 0.9800 ? C4 H4A . 0.9800 ? C4 H4B . 0.9800 ? C4 H4C . 0.9800 ? C3 H3A . 0.9800 ? C3 H3B . 0.9800 ? C3 H3C . 0.9800 ? S1A C5A . 1.767(16) ? O1A C5A . 1.209(17) ? C1A C2A . 1.57(2) ? C1A C3A . 1.50(2) ? C1A C4A . 1.55(2) ? C1A C5A . 1.553(19) ? C2A H2AA . 0.9800 ? C2A H2AB . 0.9800 ? C2A H2AC . 0.9800 ? C3A H3AA . 0.9800 ? C3A H3AB . 0.9800 ? C3A H3AC . 0.9800 ? C4A H4AA . 0.9800 ? C4A H4AB . 0.9800 ? C4A H4AC . 0.9800 ? 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 O3 H3 O5 2_565 0.84 1.96 2.802(4) 174.7 yes 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 O3 C8 C9 C10 . . . . 78.4(4) ? O3 C8 C9 C13 . . . . -163.7(4) ? O3 C8 C9 C14 . . . . -36.2(5) ? O3 C8 C12 C11 . . . . -92.8(4) ? O3 C8 C7 O2 . . . . -150.6(4) ? O3 C8 C7 C6 . . . . 33.2(5) ? O4 C15 C14 C9 . . . . 77.5(4) ? O4 C15 C16 C18 . . . . 51.7(4) ? O4 C15 C16 C17 . . . . -82.2(4) ? O5 C24 C25 C26 . . . . -147.6(4) ? C19 C23 C24 O5 . . . . 177.9(4) ? C19 C23 C24 C25 . . . . -4.1(7) ? C19 C18 C16 C15 . . . . 170.8(3) ? C19 C18 C16 C17 . . . . -54.7(4) ? C23 C19 C18 C26 . . . . -14.2(5) ? C23 C19 C18 C22 . . . . 104.7(5) ? C23 C19 C18 C16 . . . . -132.7(4) ? C23 C19 C20 C21 . . . . 133.4(4) ? C23 C24 C25 C26 . . . . 34.4(6) ? C10 C17 C16 C18 . . . . 177.5(3) ? C10 C17 C16 C15 . . . . -48.4(4) ? C10 C9 C14 C15 . . . . 55.9(4) ? C10 C11 C12 C8 . . . . 4.4(5) ? C26 C18 C16 C15 . . . . 52.0(4) ? C26 C18 C16 C17 . . . . -173.5(3) ? C21 C17 C16 C18 . . . . 57.3(4) ? C21 C17 C16 C15 . . . . -168.5(3) ? C18 C19 C23 C24 . . . . -6.6(7) ? C18 C19 C20 C21 . . . . -49.9(5) ? C18 C26 C25 C24 . . . . -56.1(5) ? C8 C9 C14 C15 . . . . 166.8(3) ? C17 C10 C9 C8 . . . . 174.8(3) ? C17 C10 C9 C13 . . . . 59.5(5) ? C17 C10 C9 C14 . . . . -63.7(4) ? C17 C10 C11 C12 . . . . -158.0(4) ? C17 C21 C20 C19 . . . . 49.7(5) ? C9 C10 C17 C21 . . . . 179.7(3) ? C9 C10 C17 C16 . . . . 59.8(4) ? C9 C10 C11 C12 . . . . -30.4(4) ? C9 C8 C12 C11 . . . . 22.6(5) ? C9 C8 C7 O2 . . . . 89.9(5) ? C9 C8 C7 C6 . . . . -86.4(5) ? C22 C18 C16 C15 . . . . -70.9(4) ? C22 C18 C16 C17 . . . . 63.5(4) ? C11 C10 C17 C21 . . . . -56.7(5) ? C11 C10 C17 C16 . . . . -176.6(4) ? C11 C10 C9 C8 . . . . 44.0(4) ? C11 C10 C9 C13 . . . . -71.3(4) ? C11 C10 C9 C14 . . . . 165.5(3) ? C20 C19 C23 C24 . . . . 169.9(4) ? C20 C19 C18 C26 . . . . 169.2(4) ? C20 C19 C18 C22 . . . . -72.0(4) ? C20 C19 C18 C16 . . . . 50.7(5) ? C20 C21 C17 C10 . . . . -172.5(3) ? C20 C21 C17 C16 . . . . -53.0(5) ? C12 C8 C9 C10 . . . . -40.1(4) ? C12 C8 C9 C13 . . . . 77.8(4) ? C12 C8 C9 C14 . . . . -154.8(4) ? C12 C8 C7 O2 . . . . -25.9(6) ? C12 C8 C7 C6 . . . . 157.8(4) ? C6 S1 C5 O1 . . . . -8.4(6) ? C6 S1 C5 C1 . . . . 169.9(5) ? C6 S1A C5A O1A . . . . 4(2) ? C6 S1A C5A C1A . . . . 179.1(15) ? C13 C9 C14 C15 . . . . -67.5(5) ? C25 C26 C18 C19 . . . . 45.3(5) ? C25 C26 C18 C22 . . . . -71.9(4) ? C25 C26 C18 C16 . . . . 162.7(3) ? C14 C15 C16 C18 . . . . 177.0(3) ? C14 C15 C16 C17 . . . . 43.2(5) ? C7 C8 C9 C10 . . . . -160.8(4) ? C7 C8 C9 C13 . . . . -42.9(5) ? C7 C8 C9 C14 . . . . 84.5(5) ? C7 C8 C12 C11 . . . . 143.9(4) ? C7 C6 S1 C5 . . . . -90.2(4) ? C7 C6 S1A C5A . . . . 81.0(8) ? C16 C15 C14 C9 . . . . -47.5(5) ? S1 C6 C7 O2 . . . . 30.1(6) ? S1 C6 C7 C8 . . . . -153.6(3) ? C2 C1 C5 S1 . . . . -106.9(8) ? C2 C1 C5 O1 . . . . 71.4(10) ? C4 C1 C5 S1 . . . . 134.2(6) ? C4 C1 C5 O1 . . . . -47.5(9) ? C3 C1 C5 S1 . . . . 11.9(7) ? C3 C1 C5 O1 . . . . -169.8(6) ? S1A C6 C7 O2 . . . . -27.2(6) ? S1A C6 C7 C8 . . . . 149.1(4) ? C2A C1A C5A S1A . . . . 92(3) ? C2A C1A C5A O1A . . . . -93(3) ? C3A C1A C5A S1A . . . . -149.7(18) ? C3A C1A C5A O1A . . . . 25(3) ? C4A C1A C5A S1A . . . . -21(2) ? C4A C1A C5A O1A . . . . 154(2) ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 1 0 0 1.32003 1.30293 -1 0 0 -0.5112 2.24972 -2 0 0 6767.16 499.349 2 0 0 6144.19 498.7 2 0 0 5866.98 499.827 3 0 0 6.13436 8.43244 -3 0 0 3.00875 5.33498 3 0 0 5.87059 4.89225 3 0 0 20.4661 7.98723 -4 0 0 70.3621 10.3054 -5 0 0 0.01148 4.97145 -5 0 0 7.27419 5.54685 -5 0 0 3.79916 5.63224 -5 0 0 10.5168 8.8301 -6 0 0 25.4077 7.64152 -6 0 0 17.6635 6.94199 -7 0 0 2.16568 4.07671 -7 0 0 4.10136 4.2484 -7 0 0 9.6639 5.09751 0 1 0 -0.0314 0.41294 0 -1 0 -0.4494 0.66937 0 1 0 -0.454 0.59783 0 -1 0 0.28995 0.68188 0 1 0 0.68527 1.18841 0 -1 0 0.10511 0.54948 1 -1 0 1050.53 88.7569 -1 1 0 1043.06 87.9367 -1 1 0 1155.56 88.0342 1 -1 0 1027.63 87.9539 1 -1 0 1122.3 88.1026 -1 -1 0 1198.54 88.638 -2 1 0 533.764 41.2123 2 -1 0 523.869 40.7326 2 -1 0 466.653 42.1898 2 1 0 505.028 40.9314 -2 -1 0 508.503 41.7185 2 -1 0 437.878 41.3751 3 -1 0 322.758 38.9985 3 1 0 363.213 34.0305 3 1 0 412.508 32.5505 3 -1 0 348.655 34.256 3 -1 0 421.973 32.35 -4 1 0 67.8578 10.2965 -4 -1 0 91.9464 17.09 4 -1 0 79.6878 21.6212 -4 -1 0 66.5371 10.346 -4 -1 0 86.6747 11.1135 -4 -1 0 55.646 10.9605 -4 -1 0 69.9611 12.9881 -4 1 0 66.5658 10.8757 4 1 0 64.7252 17.9946 -4 1 0 64.2787 9.97912 -4 1 0 45.8309 14.9217 -5 -1 0 10.6541 6.24221 -5 1 0 21.324 15.8446 -5 -1 0 6.24557 8.22271 -5 -1 0 29.7174 8.59288 -5 1 0 31.6168 8.26077 -5 1 0 21.1436 6.95162 -6 1 0 60.8325 8.75714 -6 -1 0 62.9852 8.53117 -6 -1 0 37.7832 7.93015 -6 -1 0 32.7342 9.59515 -6 1 0 49.7871 8.61597 -7 1 0 28.864 6.4326 -7 -1 0 18.4289 6.5627 -7 1 0 28.341 5.84155 -7 1 0 27.1133 5.46073 -7 -1 0 32.1463 5.88157 -7 -1 0 33.1545 6.78008 0 -2 0 1437.61 130.93 0 -2 0 1863.11 131.486 0 2 0 1476.94 130.945 0 -2 0 1734.17 131.018 0 2 0 1700.11 131.401 1 -2 0 8707.84 744.924 -1 -2 0 9999.99 744.959 2 -2 0 240.165 20.3612 -2 2 0 254.447 20.4613 -2 -2 0 251.116 21.8203 2 -2 0 241.677 21.1481 2 -2 0 197.768 21.755 3 2 0 67.6356 9.03359 -3 2 0 83.6757 9.95922 3 -2 0 53.4472 10.8697 3 2 0 66.3748 10.8111 3 -2 0 77.4888 9.38147 -4 -2 0 18.1869 6.73233 -4 2 0 9.66039 6.25506 4 2 0 5.5899 11.1914 -4 -2 0 5.54514 9.96827 -4 2 0 17.685 6.05154 -4 -2 0 17.9535 7.51043 -4 2 0 19.8937 7.16259 4 -2 0 14.7963 10.7732 -4 -2 0 21.4239 7.01598 -4 -2 0 5.76735 7.99812 -4 -2 0 35.6978 10.7872 -5 -2 0 27.201 9.93379 -5 2 0 36.1241 8.43013 -5 2 0 32.2504 7.55233 -5 -2 0 21.5213 6.26018 -5 -2 0 48.5767 9.08523 -6 -2 0 53.3089 7.45437 -6 2 0 45.5461 7.08418 -6 2 0 34.4016 8.5441 -6 -2 0 50.3411 7.4476 -6 -2 0 39.3931 9.58643 -6 2 0 34.9127 8.13502 -7 2 0 -0.8265 3.89112 -7 -2 0 7.10942 4.25456 -7 2 0 4.97612 4.78893 -7 -2 0 11.2266 7.57656 -7 2 0 3.89561 3.72692 0 -3 0 -0.0122 1.72116 0 -3 0 1.88482 2.34922 0 3 0 0.76526 2.44965 0 -3 0 -0.6617 3.04103 0 -3 0 0.58921 1.62017 0 3 0 0.10989 1.68367 -1 -3 0 8471.83 626.184 -1 3 0 7746.79 625.551 1 -3 0 8010.13 625.525 1 -3 0 8224.54 625.609 1 -3 0 6830.26 626.073 -2 3 0 705.181 55.1809 2 -3 0 741.861 55.23 -2 -3 0 572.588 56.0488 3 3 0 114.656 15.8712 -3 -3 0 183.011 17.2604 3 3 0 134.463 14.9827 3 -3 0 150.296 15.3087 3 -3 0 186.331 20.0093 -3 3 0 166.789 15.6891 -4 3 0 51.1684 8.94012 -4 3 0 44.6902 9.42316 -4 -3 0 38.9812 11.0736 -4 -3 0 39.2876 9.0191 4 -3 0 69.89 19.5409 4 3 0 66.6691 19.9616 4 3 0 33.6105 14.448 -4 -3 0 35.2357 9.04784 -4 -3 0 44.3577 11.6264 -4 -3 0 63.3414 10.5248 -4 -3 0 43.6144 10.9061 -5 -3 0 18.5295 7.28979 -5 -3 0 12.9856 6.70105 -5 3 0 -1.3459 5.39377 -5 -3 0 4.00538 5.62689 -5 3 0 6.33759 5.45856 -5 -3 0 -15.041 10.4506 -5 3 0 2.11115 5.23391 -5 -3 0 3.58808 5.6162 -6 -3 0 9.24178 4.66646 -6 -3 0 5.08142 4.70683 -6 3 0 3.5295 4.73163 -6 -3 0 -2.0636 6.39621 -6 -3 0 2.98049 5.35329 -6 3 0 5.94814 4.38775 -7 3 0 7.63979 3.96412 -7 -3 0 17.6029 5.78119 -7 3 0 21.9949 5.85036 -7 3 0 11.1334 4.07675 -7 -3 0 29.4945 7.01511 0 4 0 469.41 40.6183 0 -4 0 440.19 40.4868 0 -4 0 537.11 40.6665 0 -4 0 593.07 41.9562 0 -4 0 452.571 40.516 -1 4 0 21.918 5.21042 2 -4 0 26.9494 7.30213 -2 -4 0 12.352 4.93342 -2 4 0 20.3594 4.89464 2 -4 0 23.8809 6.33374 -2 4 0 26.2574 8.99592 2 4 0 19.2173 6.09588 2 -4 0 17.4511 5.86204 3 -4 0 1941.72 151.847 3 -4 0 1852.66 154.889 3 4 0 1819.53 153.74 3 4 0 2073.12 153.077 -3 4 0 1881.01 152.337 -3 -4 0 1774 153.684 3 4 0 1830.78 152.381 4 -4 0 1.11756 11.3154 -4 -4 0 7.54157 5.24418 4 4 0 3.32144 15.1179 -4 4 0 0.55491 5.31698 -4 -4 0 -2.5867 7.33374 -4 -4 0 -2.917 6.83882 -4 4 0 13.646 14.3767 -4 -4 0 4.36711 7.45944 -4 4 0 6.69056 5.96494 -4 -4 0 6.48644 5.82303 -4 -4 0 -1.96 7.12017 -4 -4 0 11.6395 7.11216 4 4 0 -1.6962 13.3 -5 4 0 249.37 21.1663 -5 -4 0 249.885 21.4969 -5 -4 0 227.783 21.2933 -5 4 0 211.509 21.6909 -5 4 0 234.596 21.7805 -5 -4 0 206.686 21.7619 -5 -4 0 191.016 21.4973 -6 -4 0 36.6634 7.31004 -6 4 0 51.6233 8.2182 -6 4 0 57.1153 6.8551 -6 -4 0 46.3221 7.26609 -6 -4 0 39.3677 13.5685 -6 4 0 52.1398 9.27042 -6 -4 0 58.0362 8.68097 -7 -4 0 7.9163 4.70483 -7 4 0 5.36476 3.84426 0 -5 0 -3.1626 3.59191 0 5 0 -0.1098 2.65267 0 -5 0 0.96153 2.2868 0 5 0 -1.9384 3.6349 0 -5 0 1.22297 2.53946 1 5 0 550.93 41.7578 -1 -5 0 512.925 43.1231 1 -5 0 486.061 42.9381 -1 5 0 564.03 42.992 -1 5 0 503.64 42.5331 1 5 0 462.327 43.5332 1 -5 0 496.541 43.181 1 5 0 561.226 41.7657 -1 5 0 466.365 42.7405 2 -5 0 110.497 11.8105 2 5 0 109.465 12.4047 2 -5 0 72.123 11.8521 -2 5 0 101.494 11.5861 -2 -5 0 102.94 12.3226 -2 5 0 82.8258 11.8781 -3 5 0 153.58 14.3653 -3 -5 0 137.972 16.5691 3 -5 0 160.512 17.9263 -3 5 0 112.046 15.6992 3 5 0 123.245 17.3811 -3 5 0 119.43 15.5424 -4 -5 0 91.7158 13.0661 -4 5 0 70.5805 10.3799 -4 -5 0 50.6255 10.8132 -4 5 0 53.4798 18.6071 -4 -5 0 76.2713 10.3676 -4 -5 0 79.4494 11.3425 4 5 0 75.4622 26.1712 -4 -5 0 75.8405 10.2644 -4 -5 0 60.5089 11.1101 -4 -5 0 80.9705 13.8939 -4 5 0 72.9812 10.0674 -5 -5 0 7.6802 6.29843 -5 5 0 9.35905 4.87042 -5 -5 0 13.096 5.51459 -5 5 0 7.56336 5.36621 -5 5 0 1.05781 4.76957 -5 -5 0 7.4562 6.51266 -5 -5 0 9.06747 6.22052 -6 -5 0 -8.6038 5.36062 -6 -5 0 -3.817 6.56526 -6 5 0 -5.2952 3.69726 -6 5 0 2.82535 5.30634 -6 -5 0 2.69383 6.23327 -6 -5 0 3.40737 5.05409 -6 -5 0 1.44088 4.51541 0 6 0 52.905 7.21662 0 -6 0 43.5261 6.6681 0 -6 0 49.819 6.51255 0 6 0 43.013 8.33351 1 -6 0 880.245 73.8321 1 -6 0 899.262 74.113 1 6 0 856.113 74.5745 -1 6 0 916.403 73.2341 -1 6 0 753.375 74.716 -1 -6 0 881.519 73.8118 1 6 0 986.863 72.4446 -1 6 0 991.641 74.0598 2 -6 0 1585.67 111.497 2 6 0 1213.67 109.826 2 6 0 1276.2 109.894 2 6 0 1519.84 113.111 2 -6 0 1183.43 112.117 -2 -6 0 1363.37 112.081 -2 6 0 1430.89 110.639 -2 6 0 1344.08 111.341 -2 6 0 1374.68 110.681 -3 6 0 30.0568 8.25422 3 6 0 46.9417 10.1643 -3 -6 0 28.2213 9.64012 -3 6 0 31.1036 7.21463 -3 -6 0 29.0384 7.44569 -3 -6 0 32.6626 8.79179 -3 6 0 39.4054 8.83717 3 6 0 16.3176 8.68621 -3 -6 0 30.0918 11.2423 -3 6 0 26.916 9.73102 3 -6 0 56.6981 13.3511 -4 -6 0 22.4673 6.18319 -4 -6 0 24.3268 7.49395 4 6 0 -0.8132 19.7472 -4 6 0 8.95722 16.8231 -4 -6 0 24.1333 10.151 -4 -6 0 21.8497 6.65097 -4 -6 0 23.7699 7.15655 4 -6 0 -1.0007 15.4171 -4 -6 0 42.0468 11.1174 -5 6 0 1.44104 5.04335 -5 -6 0 13.5999 6.52562 -5 6 0 27.5352 6.37215 -5 6 0 11.3533 13.3688 -5 -6 0 20.5777 7.10673 -5 -6 0 13.6751 6.78679 -5 -6 0 24.2896 7.54702 -5 -6 0 9.10441 6.44066 -6 -6 0 0.0485 5.48246 -6 -6 0 0.12923 4.53974 -6 6 0 0.24158 4.51777 -6 6 0 6.80758 4.03528 -6 -6 0 0.08075 6.40422 -6 6 0 1.76884 3.64437 0 7 0 -3.3242 5.08694 0 -7 0 1.21872 2.93565 0 7 0 2.09934 4.3097 0 -7 0 -2.5739 3.22322 0 7 0 -0.4081 4.07465 0 -7 0 -5.2019 3.64167 -1 7 0 493.618 38.4627 -1 7 0 421.527 37.0711 1 7 0 439.542 39.1799 1 -7 0 469.563 39.3388 -1 -7 0 448.927 38.1481 -1 7 0 358.523 38.2041 2 -7 0 323.104 33.592 2 7 0 333.827 33.4162 -2 -7 0 357.99 33.0312 -2 7 0 346.118 31.6638 -2 7 0 380.05 31.2719 -2 7 0 401.309 31.1793 3 -7 0 41.7655 13.6117 3 7 0 34.1425 13.9789 -3 -7 0 48.1858 8.76271 -3 -7 0 32.5324 9.69015 -3 7 0 39.7302 13.3221 -3 7 0 54.5614 10.2648 -3 -7 0 31.3044 9.8382 -3 7 0 43.6193 7.84431 -3 -7 0 36.5479 10.1377 -3 7 0 35.5576 8.24334 -3 7 0 56.6463 9.65114 -3 -7 0 33.6313 9.52794 -4 -7 0 236.426 31.8666 -4 -7 0 300.317 29.0793 -4 -7 0 224.575 28.2548 -4 7 0 257.151 23.9614 4 7 0 228.655 42.6658 4 -7 0 241.073 37.2752 -4 7 0 261.711 33.2296 -4 -7 0 269.463 24.2677 -4 7 0 247.896 24.9336 -4 -7 0 264.71 24.6358 -4 -7 0 281.969 24.3208 -4 -7 0 315.34 25.8059 -5 -7 0 11.681 5.90883 -5 7 0 3.68767 4.37724 -5 7 0 2.69941 11.7714 -5 -7 0 6.5962 5.52278 -5 -7 0 0.64318 6.43339 -5 -7 0 14.7133 5.6991 -5 7 0 7.71382 5.12517 -5 -7 0 -4.734 6.70098 -5 7 0 0.64649 5.05121 -6 -7 0 2.02631 5.21006 -6 7 0 2.44627 3.46464 -6 -7 0 0.76558 4.99202 -6 -7 0 1.40868 6.25604 -6 7 0 1.71814 4.41323 -6 7 0 0.95463 3.86566 -6 -7 0 1.21613 4.4783 0 8 0 98.2985 12.2965 0 8 0 78.1958 12.369 0 -8 0 104.684 10.5068 0 -8 0 77.8186 9.73754 0 -8 0 72.0944 9.66256 1 -8 0 133.097 15.239 -1 -8 0 159.06 16.2221 -1 8 0 153.734 16.1192 -1 8 0 142.619 14.5758 1 8 0 154.085 17.2906 -1 8 0 141.877 15.1561 1 8 0 142.753 13.8688 2 8 0 171.741 20.2521 -2 8 0 166.584 17.983 -2 8 0 190.098 16.8599 -2 -8 0 155.815 18.5133 -3 8 0 180.98 17.5598 -3 -8 0 164.769 16.8672 -3 -8 0 178.812 17.1803 -3 -8 0 190.333 17.794 3 8 0 157.424 23.5972 -3 -8 0 157.465 19.4551 -3 8 0 139.404 16.3437 -3 8 0 186.945 17.3428 3 -8 0 192.158 24.1479 -3 -8 0 160.738 20.9378 -3 -8 0 184.822 17.1984 -3 8 0 152.763 19.1286 4 8 0 77.3666 30.5319 -4 -8 0 81.5194 11.8919 -4 8 0 78.1461 11.61 -4 -8 0 79.777 12.6528 -4 -8 0 83.2991 16.8561 -4 -8 0 91.2287 11.4529 -4 -8 0 90.4882 11.6923 -4 8 0 91.3604 15.1929 -4 8 0 102.065 10.8181 4 -8 0 103.046 31.629 -4 -8 0 88.0186 11.3548 -5 8 0 50.6288 16.8429 -5 8 0 55.0442 8.64096 -5 -8 0 68.5685 11.4034 -5 -8 0 56.1889 11.1489 -5 8 0 39.1957 8.5795 -5 8 0 54.6985 7.70223 -5 -8 0 51.2353 9.17402 -5 -8 0 57.5184 8.45628 -5 -8 0 36.5894 8.41348 -6 -8 0 0.40751 4.56098 -6 -8 0 -2.3508 6.0483 -6 -8 0 -2.515 4.59911 -6 8 0 1.90878 3.55865 -6 8 0 -2.6023 3.49013 -6 8 0 4.60945 4.39404 -6 -8 0 -2.0359 6.61934 0 9 0 -11.486 6.95855 0 -9 0 -7.5449 4.63793 0 -9 0 3.29269 4.24068 0 9 0 -2.0885 5.15946 0 -9 0 -2.9731 3.68745 1 9 0 32.3065 10.4392 -1 9 0 30.2861 9.42379 -1 9 0 55.625 9.04902 -1 9 0 45.3731 7.71459 -1 -9 0 43.2098 9.04482 -2 -9 0 289.476 31.0087 -2 9 0 330.562 28.4241 2 -9 0 351.514 32.1455 -2 -9 0 334.435 30.1982 -2 9 0 312.943 30.5768 -2 9 0 315.359 30.479 -2 9 0 326.129 28.7371 2 9 0 304.105 32.2318 -2 -9 0 322.707 28.7846 -2 9 0 347.613 29.335 3 -9 0 142.322 24.515 -3 9 0 180.736 16.837 -3 -9 0 180.352 17.2673 -3 9 0 205.524 19.9846 -3 -9 0 167.86 17.3208 -3 -9 0 163.199 21.1123 -3 9 0 142.541 17.0564 3 9 0 204.817 26.9553 -3 -9 0 179.546 17.3816 -3 -9 0 168.049 20.3259 -3 9 0 181.15 18.3224 -4 9 0 57.1554 8.23094 -4 -9 0 45.1458 9.08633 -4 -9 0 50.4141 9.80919 -4 9 0 50.7769 9.69953 -4 -9 0 61.5936 8.91085 -4 -9 0 73.7371 13.8442 4 9 0 21.9276 38.7197 -4 -9 0 55.1949 9.18924 -4 9 0 84.6293 13.8113 -4 -9 0 55.4004 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11.5053 5.69198 0 -2 24 15.9289 5.35606 0 -2 -24 21.1076 6.60607 0 -2 -24 13.1598 5.13765 0 2 24 30.2983 8.58755 1 -2 24 30.1732 5.24068 1 2 -24 30.9831 8.94842 -1 -2 -24 27.5089 6.04997 1 2 -24 28.6714 7.8595 -1 -2 -24 28.7026 7.07653 -1 2 -24 18.3971 6.57627 1 2 24 22.7663 4.5677 1 -2 -24 23.5681 7.1673 1 -2 -24 18.9392 6.71503 -1 2 -24 26.7928 8.44815 0 -3 24 46.3291 6.48769 0 3 -24 45.421 10.7648 0 3 -24 37.1256 8.15922 0 3 24 39.0582 8.03867 0 -3 -24 45.0574 8.26275 0 -3 -24 52.4017 7.61478 -1 -3 -24 22.2876 5.74054 -1 -3 -24 19.8531 6.93962 1 3 -24 18.1953 7.01045 1 3 -24 30.3679 8.832 1 -3 24 10.666 3.91306 -1 3 -24 29.0931 7.43737 1 -3 -24 13.8422 5.9611 1 3 24 13.2554 4.71306 1 -3 -24 9.01952 5.17551 0 4 -24 7.19626 5.39938 0 -4 -24 1.88205 4.13543 0 4 -24 7.63094 8.03651 0 -4 -24 5.07868 4.30427 0 -4 24 -0.069 3.62983 -1 -4 -24 51.5433 10.2683 1 4 -24 75.3298 9.97083 1 4 -24 78.9138 10.0501 1 -4 24 72.6033 7.90157 -1 -4 -24 59.5384 8.34324 1 -4 -24 52.122 8.22759 -1 4 -24 60.1253 9.28682 1 4 24 55.8873 7.91833 1 -4 -24 58.3292 8.839 0 -5 24 58.0445 7.41742 0 5 -24 70.1916 10.4379 0 -5 -24 62.3325 8.0272 0 5 -24 67.8794 9.73442 0 -5 -24 53.4668 9.00007 1 5 -24 35.96 7.67845 -1 -5 -24 31.1896 6.06728 1 5 -24 47.357 8.64618 1 -5 24 39.6432 5.93142 -1 5 -24 33.1519 14.3826 1 -5 -24 37.9131 7.75422 -1 5 -24 33.1374 7.48271 1 5 24 27.2675 6.00486 1 -5 -24 53.3753 9.3578 0 6 -24 10.8859 7.3584 0 6 -24 6.61902 5.16694 0 -6 -24 12.515 6.30297 0 -6 -24 9.68333 4.35304 0 0 25 2.55662 5.80926 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.89(4) 2 0.11(4) _cod_database_fobs_code 2243875