#------------------------------------------------------------------------------ #$Date: 2015-07-11 01:45:57 +0300 (Sat, 11 Jul 2015) $ #$Revision: 143730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/48/7054808.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_7054808 loop_ _publ_author_name 'Adokoh, Christian K.' 'Obuah, Collins' 'Kinfe, Henok H.' 'Zinyemba, Orpah' 'Darkwa, James' _publ_section_title ; Novel bio-friendly and non-toxic thiocarbohydrate stabilizers of gold nanoparticles ; _journal_issue 7 _journal_name_full 'New J. Chem.' _journal_page_first 5249 _journal_paper_doi 10.1039/C5NJ00293A _journal_volume 39 _journal_year 2015 _chemical_formula_moiety 'C18 H36 N2 O12 S2' _chemical_formula_sum 'C18 H36 N2 O12 S2' _chemical_formula_weight 536.61 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2014-05-27 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _audit_update_record ; 2014-05-27 deposited with the CCDC. 2015-04-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.896(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.0828(16) _cell_length_b 8.3612(12) _cell_length_c 25.823(4) _cell_measurement_temperature 100(2) _cell_volume 2389.8(6) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _diffrn_ambient_temperature 99.85 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_unetI/netI 0.0600 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 28761 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.398 _diffrn_reflns_theta_min 0.790 _exptl_absorpt_coefficient_mu 0.288 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_F_000 1144 _refine_diff_density_max 0.576 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.11(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 634 _refine_ls_number_reflns 10392 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0498 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0623P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1113 _refine_ls_wR_factor_ref 0.1343 _reflns_Friedel_coverage 0.875 _reflns_friedel_fraction_full 0.999 _reflns_friedel_fraction_max 0.996 _reflns_number_gt 7196 _reflns_number_total 10392 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c5nj00293a2.cif _cod_data_source_block sad _cod_depositor_comments 'Adding full bibliography for 7054808.cif.' _cod_database_code 7054808 _shelxl_version_number 2013-3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All O(H) groups 2.a Ternary CH refined with riding coordinates: C1A(H1Aa), C1B(H1B), C2(H2b), C3(H3b), C5(H5a), C10(H10a), C15(H15a), C17(H17a), C20(H20a), C21(H21a), C22(H22a), C23(H23a), C32(H32), C33(H33), C34(H34), C35(H35) 2.b Secondary CH2 refined with riding coordinates: C4(H4b,H4c), C8(H8a,H8b), C9(H9a,H9b), C11(H11a,H11b), C12(H12a,H12b), C14(H14a,H14b), C16(H16a,H16b), C18(H18a,H18b), C19(H19a,H19b), C25(H25a,H25b), C26(H26a,H26b), C27(H27a,H27b), C28(H28a,H28b), C29(H29a,H29b), C30(H30a, H30b), C36(H36a,H36b) 2.c Aromatic/amide H refined with riding coordinates: N1(H1a), N2(H2a), N3(H3), N4(H4) 2.d Idealised tetrahedral OH refined as rotating group: O1(H1), O2(H2), O3(H3a), O4(H4a), O5(H5), O8(H8), O9(H9), O10(H10), O11(H11), O12(H12), O13(H13), O14(H14), O15(H15), O16(H16), O17(H17), O20(H20), O21(H21), O22(H22), O23(H23), O24(H24) ; _shelx_res_file ; TITL sad in P21 #4 CELL 0.71073 11.0828 8.3612 25.8229 90 92.896 90 ZERR 4 0.0016 0.0012 0.0039 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 72 144 8 48 8 EQIV $1 +X,+Y,-1+Z L.S. 8 0 0 PLAN 10 TEMP -173.3 HTAB O1 O12_$1 HTAB O15 O17 HTAB O22 O20 REM reset to P21 #4 BOND fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM C:/Users/Collins/Desktop/Structure/Chris/sad.hkl WGHT 0.062300 BASF 0.10921 FVAR 0.10113 S1 5 0.942469 0.958715 0.972590 11.00000 0.03785 0.02821 = 0.01820 0.00524 -0.00111 -0.01537 S2 5 0.817487 0.967663 1.027234 11.00000 0.03986 0.02699 = 0.01844 -0.00410 -0.00079 0.01516 O1 4 0.997253 0.556523 0.512014 11.00000 0.01357 0.01554 = 0.01518 -0.00255 0.00222 0.00071 AFIX 147 H1 2 0.924408 0.561198 0.501438 11.00000 -1.50000 AFIX 0 O2 4 0.976363 0.452988 0.616633 11.00000 0.01324 0.00560 = 0.01430 -0.00149 0.00038 -0.00053 AFIX 147 H2 2 0.943823 0.388867 0.595129 11.00000 -1.50000 AFIX 0 O3 4 0.960007 0.883721 0.634490 11.00000 0.01330 0.00459 = 0.02367 0.00080 0.00563 -0.00133 AFIX 147 H3A 2 1.025225 0.923184 0.625255 11.00000 -1.50000 AFIX 0 O4 4 0.775697 0.696931 0.680870 11.00000 0.00649 0.01330 = 0.01955 0.00022 0.00173 -0.00110 AFIX 147 H4A 2 0.759696 0.793673 0.675054 11.00000 -1.50000 AFIX 0 O5 4 0.894302 0.941527 0.738163 11.00000 0.01654 0.00551 = 0.02178 0.00074 0.00770 0.00009 AFIX 147 H5 2 0.944071 0.993248 0.721281 11.00000 -1.50000 AFIX 0 O6 4 0.885814 0.559560 0.797985 11.00000 0.01763 0.00879 = 0.01973 0.00148 0.00387 0.00449 O7 4 0.827118 0.577971 1.195143 11.00000 0.02937 0.02073 = 0.02129 -0.00602 0.00700 -0.01491 O8 4 0.867042 0.950245 1.260662 11.00000 0.01609 0.00790 = 0.02049 0.00090 0.00607 0.00102 AFIX 147 H8 2 0.813379 1.018613 1.265744 11.00000 -1.50000 AFIX 0 O9 4 0.965903 0.690552 1.314780 11.00000 0.00926 0.01048 = 0.01714 -0.00332 0.00202 0.00210 AFIX 147 H9 2 0.990196 0.784032 1.321100 11.00000 -1.50000 AFIX 0 O10 4 0.785785 0.904974 1.365248 11.00000 0.01082 0.00640 = 0.01977 -0.00043 0.00148 0.00024 AFIX 147 H10 2 0.859746 0.922543 1.371408 11.00000 -1.50000 AFIX 0 O11 4 0.814211 0.472524 1.385303 11.00000 0.01000 0.00566 = 0.02152 -0.00162 0.00348 0.00187 AFIX 147 H11 2 0.745141 0.432301 1.380336 11.00000 -1.50000 AFIX 0 O12 4 0.756149 0.579672 1.485715 11.00000 0.01605 0.01690 = 0.01373 0.00095 0.00467 0.00415 AFIX 147 H12 2 0.715128 0.607513 1.510665 11.00000 -1.50000 AFIX 0 N1 3 0.794094 0.795921 0.812549 11.00000 0.01790 0.01023 = 0.01343 -0.00077 0.00572 0.00188 AFIX 43 H1A 2 0.784882 0.895503 0.802050 11.00000 -1.20000 AFIX 0 N2 3 0.956153 0.786875 1.187234 11.00000 0.01563 0.00930 = 0.01497 -0.00287 0.00543 -0.00307 AFIX 43 H2A 2 0.978682 0.879922 1.200387 11.00000 -1.20000 AFIX 0 C1A 1 0.812474 0.795261 1.254728 11.00000 0.01170 0.00954 = 0.01258 0.00212 0.00293 -0.00214 AFIX 13 H1AA 2 0.723223 0.806766 1.248078 11.00000 -1.20000 AFIX 0 C1B 1 0.768699 0.741944 1.350174 11.00000 0.01083 0.00872 = 0.01160 -0.00108 0.00035 0.00128 AFIX 13 H1B 2 0.680710 0.725856 1.341191 11.00000 -1.20000 AFIX 0 C2 1 0.946514 0.615006 0.601363 11.00000 0.01036 0.00315 = 0.01656 -0.00058 0.00232 -0.00027 AFIX 13 H2B 2 0.857957 0.623142 0.592244 11.00000 -1.20000 AFIX 0 C3 1 0.978721 0.719073 0.648633 11.00000 0.00718 0.00810 = 0.01411 -0.00116 0.00189 -0.00081 AFIX 13 H3B 2 1.065768 0.702616 0.659415 11.00000 -1.20000 AFIX 0 C4 1 1.017542 0.663302 0.554870 11.00000 0.01447 0.01171 = 0.01367 -0.00204 0.00493 -0.00413 AFIX 23 H4B 2 0.993771 0.772860 0.543981 11.00000 -1.20000 H4C 2 1.104805 0.664765 0.565160 11.00000 -1.20000 AFIX 0 C5 1 0.933154 0.780482 0.743313 11.00000 0.01018 0.00419 = 0.01718 -0.00089 0.00321 0.00048 AFIX 13 H5A 2 1.022444 0.777713 0.751082 11.00000 -1.20000 AFIX 0 C6 1 0.869050 0.703045 0.787714 11.00000 0.01018 0.00887 = 0.01338 0.00055 -0.00085 -0.00150 C8 1 0.757505 0.844929 0.904035 11.00000 0.01840 0.01222 = 0.01509 -0.00084 0.00635 0.00043 AFIX 23 H8A 2 0.751831 0.959344 0.894350 11.00000 -1.20000 H8B 2 0.698464 0.824362 0.930773 11.00000 -1.20000 AFIX 0 C9 1 0.884232 0.809417 0.926475 11.00000 0.01835 0.02461 = 0.01830 -0.00044 0.00315 -0.00101 AFIX 23 H9A 2 0.939629 0.801937 0.897674 11.00000 -1.20000 H9B 2 0.883820 0.704033 0.943943 11.00000 -1.20000 AFIX 0 C10 1 0.901431 0.680072 0.694175 11.00000 0.00668 0.01093 = 0.01349 -0.00022 0.00154 -0.00047 AFIX 13 H10A 2 0.916128 0.565315 0.703399 11.00000 -1.20000 AFIX 0 C11 1 0.993640 0.834744 1.095589 11.00000 0.02077 0.01675 = 0.01183 -0.00023 0.00526 -0.00437 AFIX 23 H11A 2 1.006901 0.947956 1.105559 11.00000 -1.20000 H11B 2 1.050831 0.807723 1.068681 11.00000 -1.20000 AFIX 0 C12 1 1.018824 0.727657 1.143125 11.00000 0.01645 0.01654 = 0.01288 -0.00134 0.00687 -0.00042 AFIX 23 H12A 2 0.991845 0.617210 1.134978 11.00000 -1.20000 H12B 2 1.106803 0.724895 1.151880 11.00000 -1.20000 AFIX 0 C13 1 0.867139 0.710030 1.209046 11.00000 0.01461 0.01338 = 0.01163 0.00229 0.00117 -0.00275 C14 1 0.725721 0.742408 0.856448 11.00000 0.01623 0.01321 = 0.01744 0.00093 0.00677 -0.00059 AFIX 23 H14A 2 0.744875 0.629022 0.864248 11.00000 -1.20000 H14B 2 0.638067 0.750519 0.847387 11.00000 -1.20000 AFIX 0 C15 1 0.838663 0.692662 1.303011 11.00000 0.00998 0.01258 = 0.01325 -0.00095 0.00406 -0.00096 AFIX 13 H15A 2 0.813915 0.580725 1.293902 11.00000 -1.20000 AFIX 0 C16 1 0.865300 0.814016 1.073480 11.00000 0.02233 0.02231 = 0.01578 0.00010 0.00165 -0.00266 AFIX 23 H16A 2 0.809871 0.814361 1.102366 11.00000 -1.20000 H16B 2 0.858290 0.708406 1.056256 11.00000 -1.20000 AFIX 0 C17 1 0.803035 0.636728 1.398095 11.00000 0.01091 0.00712 = 0.01447 -0.00264 0.00045 0.00324 AFIX 13 H17A 2 0.883846 0.673702 1.412358 11.00000 -1.20000 AFIX 0 C18 1 0.713911 0.662761 1.439830 11.00000 0.01175 0.01448 = 0.01196 0.00046 0.00177 0.00271 AFIX 23 H18A 2 0.706547 0.778430 1.447230 11.00000 -1.20000 H18B 2 0.633332 0.621960 1.427968 11.00000 -1.20000 AFIX 0 S3 5 0.439225 0.959138 0.970666 11.00000 0.03286 0.02765 = 0.01784 0.00407 0.00021 -0.01263 S4 5 0.313384 0.964508 1.025015 11.00000 0.03518 0.02738 = 0.01765 -0.00404 -0.00122 0.01459 O13 4 0.118202 0.701072 1.436569 11.00000 0.00660 0.01691 = 0.01799 0.00281 0.00568 0.00318 AFIX 147 H13 2 0.081855 0.656106 1.460346 11.00000 -1.50000 AFIX 0 O14 4 0.271162 0.468784 1.389030 11.00000 0.01166 0.00801 = 0.01901 0.00056 0.00279 -0.00203 AFIX 147 H14 2 0.195488 0.461395 1.387951 11.00000 -1.50000 AFIX 0 O15 4 0.294964 0.896033 1.366460 11.00000 0.01547 0.00691 = 0.01583 0.00064 0.00224 0.00118 AFIX 147 H15 2 0.277930 0.956240 1.341094 11.00000 -1.50000 AFIX 0 O16 4 0.475471 0.722407 1.316626 11.00000 0.00576 0.01213 = 0.02035 -0.00075 0.00232 0.00078 AFIX 147 H16 2 0.481377 0.811779 1.331395 11.00000 -1.50000 AFIX 0 O17 4 0.311977 0.925412 1.257896 11.00000 0.02404 0.00725 = 0.02039 0.00124 0.00394 0.00541 AFIX 147 H17 2 0.256585 0.966304 1.238831 11.00000 -1.50000 AFIX 0 O18 4 0.375463 0.540602 1.203180 11.00000 0.01756 0.00877 = 0.01820 -0.00209 0.00560 -0.00116 O19 4 0.400996 0.548294 0.803292 11.00000 0.02691 0.01378 = 0.02303 0.00414 0.00695 0.00492 O20 4 0.427250 0.925298 0.739220 11.00000 0.02617 0.00775 = 0.01789 -0.00359 0.00319 -0.00555 AFIX 147 H20 2 0.475815 0.976089 0.759097 11.00000 -1.50000 AFIX 0 O21 4 0.284308 0.663972 0.688543 11.00000 0.00907 0.01484 = 0.01864 -0.00418 0.00353 -0.00590 AFIX 147 H21 2 0.262570 0.578707 0.673610 11.00000 -1.50000 AFIX 0 O22 4 0.427984 0.899251 0.636584 11.00000 0.01356 0.00794 = 0.01760 -0.00053 0.00130 0.00091 AFIX 147 H22 2 0.435283 0.954919 0.663640 11.00000 -1.50000 AFIX 0 O23 4 0.475725 0.482049 0.604412 11.00000 0.01418 0.00960 = 0.02137 -0.00154 0.00174 0.00031 AFIX 147 H23 2 0.551458 0.477528 0.607548 11.00000 -1.50000 AFIX 0 O24 4 0.624635 0.717330 0.557430 11.00000 0.01192 0.01704 = 0.01668 -0.00570 0.00617 -0.00450 AFIX 147 H24 2 0.647255 0.788191 0.578842 11.00000 -1.50000 AFIX 0 N3 3 0.446259 0.788304 1.185870 11.00000 0.01913 0.00734 = 0.01385 -0.00113 0.00676 0.00064 AFIX 43 H3 2 0.446093 0.889894 1.194772 11.00000 -1.20000 AFIX 0 N4 3 0.299057 0.782719 0.810482 11.00000 0.01799 0.00929 = 0.01288 0.00153 0.00579 0.00174 AFIX 43 H4 2 0.288503 0.879305 0.797492 11.00000 -1.20000 AFIX 0 C19 1 0.245549 0.691135 1.447631 11.00000 0.00987 0.01432 = 0.01347 -0.00119 0.00282 0.00045 AFIX 23 H19A 2 0.262710 0.616952 1.476964 11.00000 -1.20000 H19B 2 0.277759 0.797842 1.457573 11.00000 -1.20000 AFIX 0 C20 1 0.305945 0.631465 1.400019 11.00000 0.00832 0.00930 = 0.01468 0.00019 0.00051 -0.00082 AFIX 13 H20A 2 0.395427 0.634710 1.407193 11.00000 -1.20000 AFIX 0 C21 1 0.274632 0.734037 1.351560 11.00000 0.00796 0.00903 = 0.01551 0.00018 0.00141 -0.00063 AFIX 13 H21A 2 0.187202 0.719511 1.341114 11.00000 -1.20000 AFIX 0 C22 1 0.350851 0.684466 1.306474 11.00000 0.00710 0.01158 = 0.01363 0.00098 0.00390 0.00365 AFIX 13 H22A 2 0.344738 0.565551 1.303140 11.00000 -1.20000 AFIX 0 C23 1 0.305074 0.756596 1.254453 11.00000 0.01095 0.00773 = 0.01746 0.00373 0.00273 0.00365 AFIX 13 H23A 2 0.218776 0.724873 1.247496 11.00000 -1.20000 AFIX 0 C24 1 0.380279 0.688401 1.211810 11.00000 0.00878 0.00795 = 0.01312 -0.00253 -0.00043 0.00006 C25 1 0.519655 0.740350 1.143213 11.00000 0.01493 0.01555 = 0.01561 -0.00127 0.00674 0.00049 AFIX 23 H25A 2 0.503195 0.627021 1.134282 11.00000 -1.20000 H25B 2 0.606352 0.750430 1.153934 11.00000 -1.20000 AFIX 0 C26 1 0.490745 0.845760 1.095738 11.00000 0.01543 0.01769 = 0.01493 -0.00109 0.00374 -0.00023 AFIX 23 H26A 2 0.497524 0.959592 1.106027 11.00000 -1.20000 H26B 2 0.550793 0.825127 1.069423 11.00000 -1.20000 AFIX 0 C27 1 0.364948 0.814738 1.071985 11.00000 0.01800 0.02465 = 0.01797 0.00149 0.00503 -0.00380 AFIX 23 H27A 2 0.307473 0.810451 1.100081 11.00000 -1.20000 H27B 2 0.364060 0.708841 1.054820 11.00000 -1.20000 AFIX 0 C28 1 0.383940 0.808113 0.924733 11.00000 0.01796 0.02033 = 0.01667 0.00080 0.00509 0.00108 AFIX 23 H28A 2 0.440521 0.800760 0.896363 11.00000 -1.20000 H28B 2 0.383957 0.703206 0.942509 11.00000 -1.20000 AFIX 0 C29 1 0.258567 0.840217 0.901442 11.00000 0.01663 0.01714 = 0.01744 0.00026 0.00543 0.00278 AFIX 23 H29A 2 0.252354 0.954213 0.891292 11.00000 -1.20000 H29B 2 0.198963 0.820194 0.927989 11.00000 -1.20000 AFIX 0 C30 1 0.227424 0.736016 0.854020 11.00000 0.01290 0.01718 = 0.01782 -0.00263 0.00729 -0.00138 AFIX 23 H30A 2 0.243414 0.622440 0.862759 11.00000 -1.20000 H30B 2 0.140420 0.747098 0.844001 11.00000 -1.20000 AFIX 0 C31 1 0.379090 0.687794 0.789427 11.00000 0.01068 0.00927 = 0.01390 0.00060 -0.00022 -0.00212 C32 1 0.448237 0.757754 0.745282 11.00000 0.01179 0.00652 = 0.01469 -0.00029 0.00140 -0.00088 AFIX 13 H32 2 0.536510 0.740907 0.753381 11.00000 -1.20000 AFIX 0 C33 1 0.412765 0.667128 0.695301 11.00000 0.00966 0.00975 = 0.01521 -0.00057 0.00311 -0.00220 AFIX 13 H33 2 0.441998 0.554438 0.699291 11.00000 -1.20000 AFIX 0 C34 1 0.469224 0.739502 0.647668 11.00000 0.00726 0.00882 = 0.01401 0.00078 0.00096 -0.00173 AFIX 13 H34 2 0.558983 0.741643 0.653963 11.00000 -1.20000 AFIX 0 C35 1 0.438905 0.644188 0.598097 11.00000 0.00942 0.01164 = 0.01535 -0.00197 0.00239 0.00238 AFIX 13 H35 2 0.349203 0.645737 0.591568 11.00000 -1.20000 AFIX 0 C36 1 0.495758 0.718121 0.551271 11.00000 0.01577 0.01293 = 0.01340 0.00042 0.00138 0.00102 AFIX 23 H36A 2 0.470185 0.657241 0.519715 11.00000 -1.20000 H36B 2 0.466940 0.829558 0.546732 11.00000 -1.20000 AFIX 0 HKLF 4 REM sad in P21 #4 REM R1 = 0.0498 for 7196 Fo > 4sig(Fo) and 0.0838 for all 10392 data REM 634 parameters refined using 1 restraints END WGHT 0.0623 0.0000 REM Highest difference peak 0.576, deepest hole -0.323, 1-sigma level 0.073 Q1 1 0.9221 0.9629 0.9406 11.00000 0.05 0.58 Q2 1 0.8279 0.9708 1.0594 11.00000 0.05 0.56 Q3 1 0.3255 0.9700 1.0585 11.00000 0.05 0.55 Q4 1 0.4248 0.9667 0.9401 11.00000 0.05 0.50 Q5 1 0.4608 0.9482 1.0039 11.00000 0.05 0.48 Q6 1 0.3052 0.9720 0.9933 11.00000 0.05 0.48 Q7 1 0.9576 0.9601 1.0045 11.00000 0.05 0.46 Q8 1 0.7981 0.9733 0.9949 11.00000 0.05 0.44 Q9 1 1.0035 0.8043 1.1217 11.00000 0.05 0.36 Q10 1 0.2417 0.7840 0.8797 11.00000 0.05 0.35 ; _shelx_res_checksum 4427 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn S1 S 0.94247(11) 0.95871(16) 0.97259(4) 0.0282(3) Uani 1 1 d . S2 S 0.81749(11) 0.96766(16) 1.02723(4) 0.0285(3) Uani 1 1 d . O1 O 0.9973(2) 0.5565(4) 0.51201(10) 0.0147(6) Uani 1 1 d . H1 H 0.9244 0.5612 0.5014 0.022 Uiso 1 1 calc GR O2 O 0.9764(2) 0.4530(3) 0.61663(9) 0.0111(5) Uani 1 1 d . H2 H 0.9438 0.3889 0.5951 0.017 Uiso 1 1 calc GR O3 O 0.9600(2) 0.8837(3) 0.63449(11) 0.0137(6) Uani 1 1 d . H3A H 1.0252 0.9232 0.6253 0.021 Uiso 1 1 calc GR O4 O 0.7757(2) 0.6969(3) 0.68087(10) 0.0131(6) Uani 1 1 d . H4A H 0.7597 0.7937 0.6751 0.020 Uiso 1 1 calc GR O5 O 0.8943(2) 0.9415(3) 0.73816(10) 0.0144(6) Uani 1 1 d . H5 H 0.9441 0.9932 0.7213 0.022 Uiso 1 1 calc GR O6 O 0.8858(3) 0.5596(3) 0.79798(10) 0.0153(6) Uani 1 1 d . O7 O 0.8271(3) 0.5780(4) 1.19514(11) 0.0236(7) Uani 1 1 d . O8 O 0.8670(2) 0.9502(3) 1.26066(10) 0.0147(6) Uani 1 1 d . H8 H 0.8134 1.0186 1.2657 0.022 Uiso 1 1 calc GR O9 O 0.9659(2) 0.6906(3) 1.31478(10) 0.0122(6) Uani 1 1 d . H9 H 0.9902 0.7840 1.3211 0.018 Uiso 1 1 calc GR O10 O 0.7858(2) 0.9050(3) 1.36525(10) 0.0123(6) Uani 1 1 d . H10 H 0.8597 0.9225 1.3714 0.018 Uiso 1 1 calc GR O11 O 0.8142(2) 0.4725(3) 1.38530(10) 0.0123(6) Uani 1 1 d . H11 H 0.7451 0.4323 1.3803 0.018 Uiso 1 1 calc GR O12 O 0.7561(2) 0.5797(4) 1.48571(10) 0.0154(6) Uani 1 1 d . H12 H 0.7151 0.6075 1.5107 0.023 Uiso 1 1 calc GR N1 N 0.7941(3) 0.7959(4) 0.81255(12) 0.0137(7) Uani 1 1 d . H1A H 0.7849 0.8955 0.8021 0.016 Uiso 1 1 calc R N2 N 0.9562(3) 0.7869(4) 1.18723(12) 0.0131(7) Uani 1 1 d . H2A H 0.9787 0.8799 1.2004 0.016 Uiso 1 1 calc R C1A C 0.8125(4) 0.7953(5) 1.25473(14) 0.0112(8) Uani 1 1 d . H1AA H 0.7232 0.8068 1.2481 0.013 Uiso 1 1 calc R C1B C 0.7687(3) 0.7419(5) 1.35017(13) 0.0104(8) Uani 1 1 d . H1B H 0.6807 0.7259 1.3412 0.012 Uiso 1 1 calc R C2 C 0.9465(3) 0.6150(5) 0.60136(14) 0.0100(8) Uani 1 1 d . H2B H 0.8580 0.6231 0.5922 0.012 Uiso 1 1 calc R C3 C 0.9787(3) 0.7191(5) 0.64863(13) 0.0097(8) Uani 1 1 d . H3B H 1.0658 0.7026 0.6594 0.012 Uiso 1 1 calc R C4 C 1.0175(4) 0.6633(5) 0.55487(13) 0.0131(8) Uani 1 1 d . H4B H 0.9938 0.7729 0.5440 0.016 Uiso 1 1 calc R H4C H 1.1048 0.6648 0.5652 0.016 Uiso 1 1 calc R C5 C 0.9332(3) 0.7805(5) 0.74331(14) 0.0104(8) Uani 1 1 d . H5A H 1.0224 0.7777 0.7511 0.013 Uiso 1 1 calc R C6 C 0.8691(3) 0.7030(5) 0.78771(14) 0.0109(8) Uani 1 1 d . C8 C 0.7575(4) 0.8449(5) 0.90404(14) 0.0150(8) Uani 1 1 d . H8A H 0.7518 0.9593 0.8943 0.018 Uiso 1 1 calc R H8B H 0.6985 0.8244 0.9308 0.018 Uiso 1 1 calc R C9 C 0.8842(4) 0.8094(6) 0.92647(15) 0.0203(10) Uani 1 1 d . H9A H 0.9396 0.8019 0.8977 0.024 Uiso 1 1 calc R H9B H 0.8838 0.7040 0.9439 0.024 Uiso 1 1 calc R C10 C 0.9014(3) 0.6801(5) 0.69418(14) 0.0103(8) Uani 1 1 d . H10A H 0.9161 0.5653 0.7034 0.012 Uiso 1 1 calc R C11 C 0.9936(4) 0.8347(5) 1.09559(14) 0.0163(9) Uani 1 1 d . H11A H 1.0069 0.9480 1.1056 0.020 Uiso 1 1 calc R H11B H 1.0508 0.8077 1.0687 0.020 Uiso 1 1 calc R C12 C 1.0188(4) 0.7277(5) 1.14312(13) 0.0151(8) Uani 1 1 d . H12A H 0.9918 0.6172 1.1350 0.018 Uiso 1 1 calc R H12B H 1.1068 0.7249 1.1519 0.018 Uiso 1 1 calc R C13 C 0.8671(4) 0.7100(5) 1.20905(13) 0.0132(8) Uani 1 1 d . C14 C 0.7257(4) 0.7424(5) 0.85645(14) 0.0154(8) Uani 1 1 d . H14A H 0.7449 0.6290 0.8642 0.019 Uiso 1 1 calc R H14B H 0.6381 0.7505 0.8474 0.019 Uiso 1 1 calc R C15 C 0.8387(3) 0.6927(5) 1.30301(13) 0.0118(8) Uani 1 1 d . H15A H 0.8139 0.5807 1.2939 0.014 Uiso 1 1 calc R C16 C 0.8653(4) 0.8140(6) 1.07348(15) 0.0201(10) Uani 1 1 d . H16A H 0.8099 0.8144 1.1024 0.024 Uiso 1 1 calc R H16B H 0.8583 0.7084 1.0563 0.024 Uiso 1 1 calc R C17 C 0.8030(4) 0.6367(5) 1.39810(14) 0.0108(8) Uani 1 1 d . H17A H 0.8838 0.6737 1.4124 0.013 Uiso 1 1 calc R C18 C 0.7139(3) 0.6628(5) 1.43983(13) 0.0127(8) Uani 1 1 d . H18A H 0.7065 0.7784 1.4472 0.015 Uiso 1 1 calc R H18B H 0.6333 0.6220 1.4280 0.015 Uiso 1 1 calc R S3 S 0.43922(10) 0.95914(16) 0.97067(4) 0.0262(3) Uani 1 1 d . S4 S 0.31338(11) 0.96451(16) 1.02501(4) 0.0268(3) Uani 1 1 d . O13 O 0.1182(2) 0.7011(4) 1.43657(10) 0.0137(6) Uani 1 1 d . H13 H 0.0819 0.6561 1.4603 0.020 Uiso 1 1 calc GR O14 O 0.2712(2) 0.4688(3) 1.38903(10) 0.0128(6) Uani 1 1 d . H14 H 0.1955 0.4614 1.3880 0.019 Uiso 1 1 calc GR O15 O 0.2950(2) 0.8960(3) 1.36646(10) 0.0127(6) Uani 1 1 d . H15 H 0.2779 0.9562 1.3411 0.019 Uiso 1 1 calc GR O16 O 0.4755(2) 0.7224(4) 1.31663(10) 0.0127(6) Uani 1 1 d . H16 H 0.4814 0.8118 1.3314 0.019 Uiso 1 1 calc GR O17 O 0.3120(3) 0.9254(3) 1.25790(10) 0.0171(6) Uani 1 1 d . H17 H 0.2566 0.9663 1.2388 0.026 Uiso 1 1 calc GR O18 O 0.3755(2) 0.5406(3) 1.20318(10) 0.0147(6) Uani 1 1 d . O19 O 0.4010(3) 0.5483(4) 0.80329(11) 0.0210(7) Uani 1 1 d . O20 O 0.4273(3) 0.9253(3) 0.73922(10) 0.0172(6) Uani 1 1 d . H20 H 0.4758 0.9761 0.7591 0.026 Uiso 1 1 calc GR O21 O 0.2843(2) 0.6640(4) 0.68854(10) 0.0141(6) Uani 1 1 d . H21 H 0.2626 0.5787 0.6736 0.021 Uiso 1 1 calc GR O22 O 0.4280(2) 0.8993(3) 0.63658(10) 0.0130(6) Uani 1 1 d . H22 H 0.4353 0.9549 0.6636 0.020 Uiso 1 1 calc GR O23 O 0.4757(2) 0.4820(3) 0.60441(10) 0.0150(6) Uani 1 1 d . H23 H 0.5515 0.4775 0.6075 0.023 Uiso 1 1 calc GR O24 O 0.6246(2) 0.7173(4) 0.55743(10) 0.0150(6) Uani 1 1 d . H24 H 0.6473 0.7882 0.5788 0.023 Uiso 1 1 calc GR N3 N 0.4463(3) 0.7883(4) 1.18587(12) 0.0132(7) Uani 1 1 d . H3 H 0.4461 0.8899 1.1948 0.016 Uiso 1 1 calc R N4 N 0.2991(3) 0.7827(4) 0.81048(11) 0.0132(7) Uani 1 1 d . H4 H 0.2885 0.8793 0.7975 0.016 Uiso 1 1 calc R C19 C 0.2455(3) 0.6911(5) 1.44763(14) 0.0125(8) Uani 1 1 d . H19A H 0.2627 0.6170 1.4770 0.015 Uiso 1 1 calc R H19B H 0.2778 0.7978 1.4576 0.015 Uiso 1 1 calc R C20 C 0.3059(3) 0.6315(5) 1.40002(14) 0.0108(8) Uani 1 1 d . H20A H 0.3954 0.6347 1.4072 0.013 Uiso 1 1 calc R C21 C 0.2746(3) 0.7340(5) 1.35156(13) 0.0108(8) Uani 1 1 d . H21A H 0.1872 0.7195 1.3411 0.013 Uiso 1 1 calc R C22 C 0.3509(3) 0.6845(5) 1.30647(13) 0.0107(8) Uani 1 1 d . H22A H 0.3447 0.5656 1.3031 0.013 Uiso 1 1 calc R C23 C 0.3051(3) 0.7566(5) 1.25445(14) 0.0120(8) Uani 1 1 d . H23A H 0.2188 0.7249 1.2475 0.014 Uiso 1 1 calc R C24 C 0.3803(3) 0.6884(5) 1.21181(13) 0.0100(8) Uani 1 1 d . C25 C 0.5197(4) 0.7403(5) 1.14321(14) 0.0152(8) Uani 1 1 d . H25A H 0.5032 0.6270 1.1343 0.018 Uiso 1 1 calc R H25B H 0.6064 0.7504 1.1539 0.018 Uiso 1 1 calc R C26 C 0.4907(3) 0.8458(5) 1.09574(14) 0.0159(9) Uani 1 1 d . H26A H 0.4975 0.9596 1.1060 0.019 Uiso 1 1 calc R H26B H 0.5508 0.8251 1.0694 0.019 Uiso 1 1 calc R C27 C 0.3649(4) 0.8147(6) 1.07199(15) 0.0201(10) Uani 1 1 d . H27A H 0.3075 0.8105 1.1001 0.024 Uiso 1 1 calc R H27B H 0.3641 0.7088 1.0548 0.024 Uiso 1 1 calc R C28 C 0.3839(4) 0.8081(5) 0.92473(15) 0.0182(9) Uani 1 1 d . H28A H 0.4405 0.8008 0.8964 0.022 Uiso 1 1 calc R H28B H 0.3840 0.7032 0.9425 0.022 Uiso 1 1 calc R C29 C 0.2586(4) 0.8402(5) 0.90144(15) 0.0169(9) Uani 1 1 d . H29A H 0.2524 0.9542 0.8913 0.020 Uiso 1 1 calc R H29B H 0.1990 0.8202 0.9280 0.020 Uiso 1 1 calc R C30 C 0.2274(3) 0.7360(6) 0.85402(14) 0.0157(8) Uani 1 1 d . H30A H 0.2434 0.6224 0.8628 0.019 Uiso 1 1 calc R H30B H 0.1404 0.7471 0.8440 0.019 Uiso 1 1 calc R C31 C 0.3791(3) 0.6878(5) 0.78943(14) 0.0113(8) Uani 1 1 d . C32 C 0.4482(3) 0.7578(5) 0.74528(14) 0.0110(8) Uani 1 1 d . H32 H 0.5365 0.7409 0.7534 0.013 Uiso 1 1 calc R C33 C 0.4128(3) 0.6671(5) 0.69530(14) 0.0115(8) Uani 1 1 d . H33 H 0.4420 0.5544 0.6993 0.014 Uiso 1 1 calc R C34 C 0.4692(3) 0.7395(5) 0.64767(13) 0.0100(8) Uani 1 1 d . H34 H 0.5590 0.7416 0.6540 0.012 Uiso 1 1 calc R C35 C 0.4389(3) 0.6442(5) 0.59810(14) 0.0121(8) Uani 1 1 d . H35 H 0.3492 0.6457 0.5916 0.014 Uiso 1 1 calc R C36 C 0.4958(3) 0.7181(5) 0.55127(14) 0.0140(8) Uani 1 1 d . H36A H 0.4702 0.6572 0.5197 0.017 Uiso 1 1 calc R H36B H 0.4669 0.8296 0.5467 0.017 Uiso 1 1 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0379(7) 0.0282(8) 0.0182(5) 0.0052(5) -0.0011(4) -0.0154(6) S2 0.0399(7) 0.0270(7) 0.0184(5) -0.0041(5) -0.0008(4) 0.0152(6) O1 0.0136(14) 0.0155(17) 0.0152(13) -0.0026(12) 0.0022(11) 0.0007(13) O2 0.0132(13) 0.0056(15) 0.0143(12) -0.0015(11) 0.0004(10) -0.0005(12) O3 0.0133(14) 0.0046(15) 0.0237(15) 0.0008(11) 0.0056(11) -0.0013(11) O4 0.0065(13) 0.0133(17) 0.0195(14) 0.0002(12) 0.0017(10) -0.0011(11) O5 0.0165(14) 0.0055(15) 0.0218(14) 0.0007(12) 0.0077(11) 0.0001(12) O6 0.0176(15) 0.0088(15) 0.0197(14) 0.0015(11) 0.0039(11) 0.0045(12) O7 0.0294(18) 0.0207(19) 0.0213(15) -0.0060(13) 0.0070(13) -0.0149(15) O8 0.0161(13) 0.0079(15) 0.0205(13) 0.0009(12) 0.0061(11) 0.0010(13) O9 0.0093(14) 0.0105(17) 0.0171(13) -0.0033(11) 0.0020(10) 0.0021(11) O10 0.0108(13) 0.0064(15) 0.0198(13) -0.0004(11) 0.0015(11) 0.0002(11) O11 0.0100(13) 0.0057(14) 0.0215(13) -0.0016(12) 0.0035(10) 0.0019(12) O12 0.0161(15) 0.0169(17) 0.0137(13) 0.0009(12) 0.0047(11) 0.0042(13) N1 0.0179(17) 0.0102(19) 0.0134(16) -0.0008(13) 0.0057(13) 0.0019(14) N2 0.0156(17) 0.0093(18) 0.0150(16) -0.0029(13) 0.0054(13) -0.0031(14) C1A 0.0117(19) 0.010(2) 0.0126(18) 0.0021(15) 0.0029(14) -0.0021(16) C1B 0.0108(18) 0.009(2) 0.0116(17) -0.0011(15) 0.0004(14) 0.0013(16) C2 0.0104(19) 0.0032(19) 0.0166(18) -0.0006(14) 0.0023(14) -0.0003(15) C3 0.0072(17) 0.008(2) 0.0141(17) -0.0012(15) 0.0019(13) -0.0008(15) C4 0.014(2) 0.012(2) 0.0137(18) -0.0020(15) 0.0049(15) -0.0041(17) C5 0.0102(18) 0.004(2) 0.0172(18) -0.0009(14) 0.0032(15) 0.0005(15) C6 0.0102(19) 0.009(2) 0.0134(17) 0.0005(15) -0.0008(14) -0.0015(16) C8 0.018(2) 0.012(2) 0.0151(19) -0.0008(16) 0.0063(15) 0.0004(17) C9 0.018(2) 0.025(3) 0.018(2) -0.0004(18) 0.0031(17) -0.0010(19) C10 0.0067(18) 0.011(2) 0.0135(17) -0.0002(15) 0.0015(13) -0.0005(15) C11 0.021(2) 0.017(2) 0.0118(18) -0.0002(16) 0.0053(16) -0.0044(18) C12 0.016(2) 0.017(2) 0.0129(17) -0.0013(16) 0.0069(15) -0.0004(18) C13 0.015(2) 0.013(2) 0.0116(17) 0.0023(16) 0.0012(14) -0.0028(17) C14 0.016(2) 0.013(2) 0.0174(18) 0.0009(16) 0.0068(15) -0.0006(18) C15 0.0100(19) 0.013(2) 0.0132(17) -0.0010(15) 0.0041(14) -0.0010(16) C16 0.022(2) 0.022(3) 0.016(2) 0.0001(18) 0.0017(17) -0.0027(19) C17 0.0109(19) 0.007(2) 0.0145(18) -0.0026(15) 0.0005(14) 0.0032(15) C18 0.0118(19) 0.014(2) 0.0120(17) 0.0005(15) 0.0018(14) 0.0027(17) S3 0.0329(6) 0.0277(7) 0.0178(5) 0.0041(5) 0.0002(4) -0.0126(6) S4 0.0352(6) 0.0274(7) 0.0176(5) -0.0040(5) -0.0012(4) 0.0146(6) O13 0.0066(13) 0.0169(17) 0.0180(13) 0.0028(12) 0.0057(10) 0.0032(12) O14 0.0117(13) 0.0080(15) 0.0190(13) 0.0006(12) 0.0028(10) -0.0020(12) O15 0.0155(14) 0.0069(15) 0.0158(13) 0.0006(11) 0.0022(11) 0.0012(12) O16 0.0058(13) 0.0121(16) 0.0204(14) -0.0007(12) 0.0023(10) 0.0008(11) O17 0.0240(16) 0.0072(15) 0.0204(14) 0.0012(12) 0.0039(11) 0.0054(13) O18 0.0176(15) 0.0088(15) 0.0182(13) -0.0021(11) 0.0056(11) -0.0012(12) O19 0.0269(17) 0.0138(17) 0.0230(15) 0.0041(12) 0.0069(12) 0.0049(14) O20 0.0262(16) 0.0078(15) 0.0179(13) -0.0036(11) 0.0032(11) -0.0055(13) O21 0.0091(14) 0.0148(17) 0.0186(14) -0.0042(12) 0.0035(11) -0.0059(12) O22 0.0136(14) 0.0079(15) 0.0176(13) -0.0005(11) 0.0013(11) 0.0009(12) O23 0.0142(14) 0.0096(16) 0.0214(13) -0.0015(12) 0.0017(11) 0.0003(12) O24 0.0119(14) 0.0170(17) 0.0167(14) -0.0057(12) 0.0062(10) -0.0045(12) N3 0.0191(18) 0.0073(18) 0.0138(16) -0.0011(13) 0.0068(13) 0.0006(14) N4 0.0180(17) 0.0093(19) 0.0129(15) 0.0015(13) 0.0058(13) 0.0017(14) C19 0.0099(19) 0.014(2) 0.0135(17) -0.0012(15) 0.0028(14) 0.0004(16) C20 0.0083(18) 0.009(2) 0.0147(18) 0.0002(15) 0.0005(14) -0.0008(15) C21 0.0080(18) 0.009(2) 0.0155(18) 0.0002(15) 0.0014(14) -0.0006(16) C22 0.0071(18) 0.012(2) 0.0136(17) 0.0010(15) 0.0039(13) 0.0036(15) C23 0.0109(19) 0.008(2) 0.0175(18) 0.0037(15) 0.0027(14) 0.0036(16) C24 0.0088(18) 0.008(2) 0.0131(17) -0.0025(14) -0.0004(13) 0.0001(15) C25 0.015(2) 0.016(2) 0.0156(18) -0.0013(16) 0.0067(15) 0.0005(18) C26 0.015(2) 0.018(2) 0.0149(19) -0.0011(16) 0.0037(15) -0.0002(17) C27 0.018(2) 0.025(3) 0.018(2) 0.0015(18) 0.0050(17) -0.0038(19) C28 0.018(2) 0.020(3) 0.0167(19) 0.0008(17) 0.0051(16) 0.0011(19) C29 0.017(2) 0.017(2) 0.017(2) 0.0003(17) 0.0054(16) 0.0028(17) C30 0.0129(19) 0.017(2) 0.0178(19) -0.0026(17) 0.0073(15) -0.0014(18) C31 0.0107(19) 0.009(2) 0.0139(17) 0.0006(15) -0.0002(14) -0.0021(16) C32 0.0118(19) 0.007(2) 0.0147(18) -0.0003(15) 0.0014(14) -0.0009(16) C33 0.0097(18) 0.010(2) 0.0152(18) -0.0006(15) 0.0031(14) -0.0022(16) C34 0.0073(17) 0.009(2) 0.0140(17) 0.0008(15) 0.0010(14) -0.0017(16) C35 0.0094(19) 0.012(2) 0.0153(18) -0.0020(15) 0.0024(14) 0.0024(16) C36 0.016(2) 0.013(2) 0.0134(17) 0.0004(16) 0.0014(14) 0.0010(17) 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 C9 S1 S2 104.38(15) C16 S2 S1 104.17(15) C6 N1 C14 123.8(4) C13 N2 C12 124.3(4) O8 C1A C13 108.8(3) O8 C1A C15 111.0(3) C13 C1A C15 107.5(3) O10 C1B C15 114.1(3) O10 C1B C17 107.5(3) C15 C1B C17 111.6(3) O2 C2 C3 106.0(3) O2 C2 C4 110.1(3) C4 C2 C3 111.7(3) O3 C3 C2 108.5(3) O3 C3 C10 108.8(3) C10 C3 C2 112.2(3) O1 C4 C2 112.1(3) O5 C5 C6 108.9(3) O5 C5 C10 112.5(3) C6 C5 C10 106.9(3) O6 C6 N1 123.6(4) O6 C6 C5 120.1(3) N1 C6 C5 116.3(3) C9 C8 C14 111.6(3) C8 C9 S1 113.9(3) O4 C10 C3 111.9(3) O4 C10 C5 108.8(3) C3 C10 C5 113.8(3) C16 C11 C12 111.4(3) N2 C12 C11 110.7(3) O7 C13 N2 125.0(4) O7 C13 C1A 119.3(4) N2 C13 C1A 115.7(4) N1 C14 C8 110.1(3) O9 C15 C1A 109.0(3) O9 C15 C1B 111.6(3) C1A C15 C1B 114.5(3) C11 C16 S2 113.8(3) O11 C17 C1B 112.6(3) O11 C17 C18 111.9(3) C18 C17 C1B 110.1(3) O12 C18 C17 108.8(3) C28 S3 S4 104.24(15) C27 S4 S3 104.05(15) C24 N3 C25 123.8(4) C31 N4 C30 123.7(3) O13 C19 C20 109.3(3) O14 C20 C19 110.3(3) O14 C20 C21 108.6(3) C19 C20 C21 112.7(3) O15 C21 C20 106.5(3) O15 C21 C22 112.2(3) C22 C21 C20 110.9(3) O16 C22 C21 111.5(3) O16 C22 C23 110.3(3) C21 C22 C23 112.9(3) O17 C23 C22 108.8(3) O17 C23 C24 112.8(3) C24 C23 C22 108.5(3) O18 C24 N3 123.6(4) O18 C24 C23 118.4(3) N3 C24 C23 117.9(3) N3 C25 C26 110.2(3) C27 C26 C25 112.1(3) C26 C27 S4 113.8(3) C29 C28 S3 114.2(3) C28 C29 C30 112.6(3) N4 C30 C29 110.8(3) O19 C31 N4 124.7(4) O19 C31 C32 118.6(4) N4 C31 C32 116.7(3) O20 C32 C31 112.0(3) O20 C32 C33 111.1(3) C31 C32 C33 108.9(3) O21 C33 C32 108.9(3) O21 C33 C34 110.8(3) C32 C33 C34 112.5(3) O22 C34 C33 112.9(3) O22 C34 C35 105.3(3) C35 C34 C33 112.6(3) O23 C35 C34 110.5(3) O23 C35 C36 110.5(3) C36 C35 C34 111.8(3) O24 C36 C35 111.2(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 S2 2.0280(18) S1 C9 1.821(4) S2 C16 1.815(4) O1 C4 1.431(4) O2 C2 1.445(5) O3 C3 1.437(5) O4 C10 1.425(4) O5 C5 1.418(4) O6 C6 1.241(5) O7 C13 1.236(5) O8 C1A 1.435(5) O9 C15 1.428(5) O10 C1B 1.428(5) O11 C17 1.419(5) O12 C18 1.432(4) N1 C6 1.326(5) N1 C14 1.465(5) N2 C12 1.451(5) N2 C13 1.326(5) C1A C13 1.529(5) C1A C15 1.529(5) C1B C15 1.533(5) C1B C17 1.550(5) C2 C3 1.527(5) C2 C4 1.523(5) C3 C10 1.525(5) C5 C6 1.523(5) C5 C10 1.547(5) C8 C9 1.521(5) C8 C14 1.525(5) C11 C12 1.534(5) C11 C16 1.516(5) C17 C18 1.514(5) S3 S4 2.0284(17) S3 C28 1.818(4) S4 C27 1.815(4) O13 C19 1.428(4) O14 C20 1.438(5) O15 C21 1.423(5) O16 C22 1.428(4) O17 C23 1.416(5) O18 C24 1.256(5) O19 C31 1.240(5) O20 C32 1.427(5) O21 C33 1.426(5) O22 C34 1.436(5) O23 C35 1.423(5) O24 C36 1.429(5) N3 C24 1.316(5) N3 C25 1.458(5) N4 C30 1.462(5) N4 C31 1.327(5) C19 C20 1.514(5) C20 C21 1.542(5) C21 C22 1.530(5) C22 C23 1.535(5) C23 C24 1.525(5) C25 C26 1.531(5) C26 C27 1.517(5) C28 C29 1.510(5) C29 C30 1.528(5) C31 C32 1.522(5) C32 C33 1.531(5) C33 C34 1.532(5) C34 C35 1.531(5) C35 C36 1.523(5) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O12 0.84 1.89 2.730(4) 173.1 1_554 O15 H15 O17 0.84 2.22 2.830(4) 130.1 . O22 H22 O20 0.84 1.97 2.660(4) 138.2 .