#------------------------------------------------------------------------------ #$Date: 2024-12-18 05:01:29 +0200 (Wed, 18 Dec 2024) $ #$Revision: 296910 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312735.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_2312735 loop_ _publ_author_name 'Zhang, Yao' 'Wang, Yan Juan' 'Tang, Yuan Yuan' 'Chen, Xiao Gang' _publ_section_title ; Crown ether inclusion compound 3,4-difluoroanilinium di(methanesulfonyl)amidate-18-crown-6 (1/1) clathrate. ; _journal_coeditor_code DG3066 _journal_issue 1 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229624011872 _journal_volume 81 _journal_year 2025 _chemical_formula_iupac 'C6 H6 F2 N +, C2 H6 N O4 S2 -, C12 H24 O6' _chemical_formula_moiety 'C6 H6 F2 N +, C2 H6 N O4 S2 -, C12 H24 O6' _chemical_formula_sum 'C20 H36 F2 N2 O10 S2' _chemical_formula_weight 566.63 _chemical_name_common ; 3,4-Difluoroanilinium--di(methanesulfonyl)amidate--18-crown-6 (1/1) ; _chemical_name_systematic '3,4-Difluoroanilinium di(methanesulfonyl)amidate--1,4,7,10,13,16-hexaoxacyclooctadecane (1/1)' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 104.6327(15) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.67269(15) _cell_length_b 15.8882(2) _cell_length_c 16.0990(2) _cell_measurement_reflns_used 14997 _cell_measurement_temperature 300.2(7) _cell_measurement_theta_max 71.6490 _cell_measurement_theta_min 3.9420 _cell_volume 2641.36(6) _computing_cell_refinement ; CrysAlis PRO (Rigaku OD, 2024) ; _computing_data_collection ; CrysAlis PRO (Rigaku OD, 2024) ; _computing_data_reduction ; CrysAlis PRO (Rigaku OD, 2024) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 300.2(7) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy--DW diffractometer with a HyPix-Arc 150 detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_unetI/netI 0.0213 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 25974 _diffrn_reflns_theta_full 66.600 _diffrn_reflns_theta_max 66.600 _diffrn_reflns_theta_min 3.974 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 2.445 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2024) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.425 _exptl_crystal_description block _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.395 _refine_diff_density_min -0.415 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 316 _refine_ls_number_reflns 4679 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0439 _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^)+(0.0636P)^2^+1.1189P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1177 _refine_ls_wR_factor_ref 0.1242 _reflns_number_gt 3810 _reflns_number_total 4679 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL zy_240926_1_300k_auto_a.res in P2(1)/c zy_240926_1_300k_auto.res created by SHELXL-2018/3 at 15:06:29 on 13-Oct-2024 REM Old TITL zy_240926_1_300k_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.171, Rweak 0.063, Alpha 0.031 REM 0.387 for 147 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N2 O8 C20 S2 CELL 1.54184 10.672692 15.888206 16.099029 90 104.6327 90 ZERR 4 0.000149 0.000205 0.000232 0 0.0015 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H F N O S UNIT 80 144 8 8 40 8 L.S. 20 PLAN 5 SIZE 0.06 0.05 0.04 TEMP 27 CONF HTAB N1 O2 HTAB N1 O4 HTAB N1 O6 MORE -1 BOND $H fmap 2 acta SHEL 999 0.84 REM REM REM WGHT 0.063600 1.118900 FVAR 0.35525 C1 1 0.691228 0.448872 0.461868 11.00000 0.08694 0.07794 = 0.05392 0.00294 -0.00391 0.02565 AFIX 23 H1A 2 0.675868 0.504160 0.482874 11.00000 -1.20000 H1B 2 0.760648 0.422265 0.504446 11.00000 -1.20000 AFIX 0 C2 1 0.572497 0.397473 0.447663 11.00000 0.10596 0.06965 = 0.06913 0.02725 0.03179 0.02513 AFIX 23 H2A 2 0.585410 0.344395 0.421229 11.00000 -1.20000 H2B 2 0.553356 0.385475 0.502244 11.00000 -1.20000 AFIX 0 C3 1 0.351721 0.392608 0.368757 11.00000 0.09316 0.05254 = 0.07987 -0.00440 0.04714 -0.01701 AFIX 23 H3A 2 0.327747 0.372642 0.419565 11.00000 -1.20000 H3B 2 0.366730 0.344039 0.336056 11.00000 -1.20000 AFIX 0 C4 1 0.246166 0.443941 0.316393 11.00000 0.06015 0.07117 = 0.08755 -0.01922 0.04046 -0.01889 AFIX 23 H4A 2 0.164560 0.414137 0.307745 11.00000 -1.20000 H4B 2 0.239248 0.496535 0.345507 11.00000 -1.20000 AFIX 0 C5 1 0.172176 0.502947 0.177214 11.00000 0.03853 0.05483 = 0.10721 -0.01377 0.00784 -0.00175 AFIX 23 H5A 2 0.156989 0.557139 0.200652 11.00000 -1.20000 H5B 2 0.092992 0.470282 0.167310 11.00000 -1.20000 AFIX 0 C6 1 0.209410 0.514842 0.095640 11.00000 0.05846 0.05385 = 0.07821 -0.01674 -0.01878 0.00528 AFIX 23 H6A 2 0.228251 0.460774 0.073556 11.00000 -1.20000 H6B 2 0.138595 0.540594 0.053430 11.00000 -1.20000 AFIX 0 C7 1 0.365991 0.581716 0.035415 11.00000 0.09220 0.06823 = 0.04198 0.00049 0.00393 0.03199 AFIX 23 H7A 2 0.299346 0.609632 -0.008055 11.00000 -1.20000 H7B 2 0.385997 0.528433 0.012301 11.00000 -1.20000 AFIX 0 C8 1 0.483458 0.634935 0.058675 11.00000 0.12286 0.05585 = 0.06108 0.01653 0.04363 0.01791 AFIX 23 H8A 2 0.505890 0.654136 0.007076 11.00000 -1.20000 H8B 2 0.467278 0.683925 0.090389 11.00000 -1.20000 AFIX 0 C9 1 0.709632 0.628027 0.125489 11.00000 0.09898 0.07992 = 0.08451 -0.00862 0.05287 -0.03233 AFIX 23 H9A 2 0.708532 0.679226 0.158118 11.00000 -1.20000 H9B 2 0.728571 0.642875 0.071494 11.00000 -1.20000 AFIX 0 C10 1 0.810096 0.569653 0.174488 11.00000 0.06822 0.09822 = 0.10949 -0.03485 0.05463 -0.02483 AFIX 23 H10A 2 0.806032 0.516612 0.144085 11.00000 -1.20000 H10B 2 0.895437 0.593736 0.180485 11.00000 -1.20000 AFIX 0 C11 1 0.879332 0.499675 0.308850 11.00000 0.03572 0.05125 = 0.14753 -0.01645 0.02023 0.00166 AFIX 23 H11A 2 0.966542 0.520764 0.315213 11.00000 -1.20000 H11B 2 0.873113 0.444775 0.281755 11.00000 -1.20000 AFIX 0 C12 1 0.852297 0.492285 0.393374 11.00000 0.04644 0.04745 = 0.11341 -0.00805 -0.02029 0.00157 AFIX 23 H12A 2 0.916935 0.456762 0.430318 11.00000 -1.20000 H12B 2 0.855833 0.547403 0.419779 11.00000 -1.20000 AFIX 0 O1 5 0.726507 0.456503 0.383433 11.00000 0.04933 0.05971 = 0.06173 -0.00713 -0.00243 0.00083 O2 5 0.466780 0.441697 0.393335 11.00000 0.06823 0.05035 = 0.06437 0.00985 0.02276 0.00288 O3 5 0.273525 0.460307 0.235672 11.00000 0.04583 0.06573 = 0.07656 -0.00580 0.02109 0.00124 O4 5 0.321061 0.567566 0.110496 11.00000 0.05786 0.05205 = 0.04832 -0.00835 0.00181 0.00750 O5 5 0.587180 0.587185 0.109831 11.00000 0.07531 0.05268 = 0.06439 0.00177 0.02810 -0.00638 O6 5 0.788168 0.555945 0.256513 11.00000 0.04417 0.06229 = 0.08793 -0.01551 0.02400 0.00061 AFIX 66 C13 1 0.518579 0.645337 0.297843 11.00000 0.04131 0.03628 = 0.03852 -0.00125 0.01196 0.00004 C14 1 0.631528 0.686069 0.341044 11.00000 0.03907 0.04891 = 0.06944 -0.01471 0.00602 0.00168 AFIX 43 H14 2 0.709133 0.656479 0.356563 11.00000 -1.20000 AFIX 65 C15 1 0.628487 0.771026 0.361051 11.00000 0.04931 0.05476 = 0.08179 -0.02539 0.01126 -0.00915 AFIX 43 H15 2 0.704058 0.798278 0.389955 11.00000 -1.20000 AFIX 65 C16 1 0.512497 0.815252 0.337857 11.00000 0.06100 0.03908 = 0.05240 -0.00851 0.01960 -0.00090 C17 1 0.399547 0.774521 0.294656 11.00000 0.04987 0.04329 = 0.04622 0.00161 0.01038 0.01053 C18 1 0.402586 0.689564 0.274649 11.00000 0.04092 0.04306 = 0.05063 -0.00431 0.00418 0.00022 AFIX 43 H18 2 0.327015 0.662312 0.245744 11.00000 -1.20000 AFIX 0 F1 3 0.507040 0.896862 0.354382 11.00000 0.08793 0.04035 = 0.09104 -0.01746 0.03115 -0.00208 F2 3 0.291364 0.818308 0.273171 11.00000 0.06392 0.06078 = 0.08899 -0.00309 0.00150 0.02366 N1 4 0.522714 0.558788 0.270986 11.00000 0.03986 0.03609 = 0.04558 0.00028 0.00893 -0.00094 AFIX 137 H1C 2 0.464130 0.550988 0.221364 11.00000 -1.20000 H1D 2 0.505335 0.524893 0.310655 11.00000 -1.20000 H1E 2 0.601222 0.547193 0.264402 11.00000 -1.20000 AFIX 0 C19 1 -0.020901 0.782999 0.309144 11.00000 0.14194 0.09117 = 0.07731 0.03319 0.04683 0.05496 AFIX 137 H19A 2 -0.096678 0.751733 0.280924 11.00000 -1.50000 H19B 2 0.022656 0.802363 0.267346 11.00000 -1.50000 H19C 2 -0.045808 0.830450 0.338254 11.00000 -1.50000 AFIX 0 C20 1 0.112841 0.752463 0.599778 11.00000 0.06130 0.06217 = 0.05293 -0.00496 0.00710 -0.00557 AFIX 137 H20A 2 0.148384 0.698150 0.618497 11.00000 -1.50000 H20B 2 0.094406 0.781999 0.647350 11.00000 -1.50000 H20C 2 0.174192 0.784069 0.577893 11.00000 -1.50000 AFIX 0 N2 4 0.001512 0.683185 0.445553 11.00000 0.05347 0.04108 = 0.05514 -0.00320 0.01006 -0.00754 O7 5 0.112160 0.648667 0.334883 11.00000 0.08195 0.06531 = 0.07915 -0.01802 0.02931 0.00811 O8 5 0.193052 0.765987 0.428245 11.00000 0.09571 0.12567 = 0.08434 -0.04072 0.04047 -0.06653 O9 5 -0.073844 0.823426 0.489813 11.00000 0.07785 0.06229 = 0.07447 0.00096 0.01714 0.02702 O10 5 -0.117030 0.691751 0.555024 11.00000 0.07470 0.10927 = 0.08964 -0.00285 0.03993 -0.03583 S1 6 0.083208 0.718215 0.383697 11.00000 0.05505 0.04591 = 0.05569 -0.00791 0.01517 -0.00685 S2 6 -0.030640 0.739974 0.518573 11.00000 0.04386 0.05339 = 0.05563 0.00008 0.01285 -0.00433 HKLF 4 REM zy_240926_1_300k_auto_a.res in P2(1)/c REM wR2 = 0.1242, GooF = S = 1.045, Restrained GooF = 1.045 for all data REM R1 = 0.0439 for 3810 Fo > 4sig(Fo) and 0.0541 for all 4679 data REM 316 parameters refined using 0 restraints END WGHT 0.0634 1.1134 REM Highest difference peak 0.395, deepest hole -0.415, 1-sigma level 0.046 Q1 1 0.1203 0.8122 0.3979 11.00000 0.05 0.39 Q2 1 0.5128 0.6658 0.2908 11.00000 0.05 0.35 Q3 1 0.0290 0.7541 0.3534 11.00000 0.05 0.31 Q4 1 0.5229 0.8028 0.3256 11.00000 0.05 0.30 Q5 1 0.4409 0.7781 0.3190 11.00000 0.05 0.28 REM The information below was added by Olex2. REM REM R1 = 0.0439 for 3810 Fo > 4sig(Fo) and 0.0541 for all 27436 data REM 316 parameters refined using n/a restraints REM Highest difference peak 0.39, deepest hole -0.41 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0541 REM R1_gt = 0.0439 REM wR_ref = 0.1242 REM GOOF = 1.045 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 27436 REM Reflections_gt = 3810 REM Parameters = 316 REM Hole = -0.41 REM Peak = 0.39 REM Flack = n/a ; _cod_data_source_file dg3066sup1.cif _cod_data_source_block zy_240926_1_300k_auto _cod_original_cell_volume 2641.37(7) _cod_database_code 2312735 _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 0.867 _shelx_estimated_absorpt_t_max 0.909 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 C C1 0.6912(3) 0.4489(2) 0.46187(18) 0.0768(9) Uani d 1 . . H H1A 0.675868 0.504160 0.482874 0.092 Uiso calc 1 . . H H1B 0.760648 0.422265 0.504446 0.092 Uiso calc 1 . . C C2 0.5725(3) 0.3975(2) 0.4477(2) 0.0798(9) Uani d 1 . . H H2A 0.585410 0.344395 0.421229 0.096 Uiso calc 1 . . H H2B 0.553356 0.385475 0.502244 0.096 Uiso calc 1 . . C C3 0.3517(3) 0.39261(17) 0.3688(2) 0.0706(8) Uani d 1 . . H H3A 0.327747 0.372642 0.419565 0.085 Uiso calc 1 . . H H3B 0.366730 0.344039 0.336056 0.085 Uiso calc 1 . . C C4 0.2462(3) 0.44394(19) 0.3164(2) 0.0690(8) Uani d 1 . . H H4A 0.164560 0.414137 0.307745 0.083 Uiso calc 1 . . H H4B 0.239248 0.496535 0.345507 0.083 Uiso calc 1 . . C C5 0.1722(2) 0.50295(17) 0.1772(2) 0.0688(8) Uani d 1 . . H H5A 0.156989 0.557139 0.200652 0.083 Uiso calc 1 . . H H5B 0.092992 0.470282 0.167310 0.083 Uiso calc 1 . . C C6 0.2094(3) 0.51484(17) 0.09564(19) 0.0700(8) Uani d 1 . . H H6A 0.228251 0.460774 0.073556 0.084 Uiso calc 1 . . H H6B 0.138595 0.540594 0.053430 0.084 Uiso calc 1 . . C C7 0.3660(3) 0.58172(18) 0.03541(16) 0.0698(8) Uani d 1 . . H H7A 0.299346 0.609632 -0.008055 0.084 Uiso calc 1 . . H H7B 0.385997 0.528433 0.012301 0.084 Uiso calc 1 . . C C8 0.4835(3) 0.63493(19) 0.05867(18) 0.0763(9) Uani d 1 . . H H8A 0.505890 0.654136 0.007076 0.092 Uiso calc 1 . . H H8B 0.467278 0.683925 0.090389 0.092 Uiso calc 1 . . C C9 0.7096(3) 0.6280(2) 0.1255(2) 0.0825(10) Uani d 1 . . H H9A 0.708532 0.679226 0.158118 0.099 Uiso calc 1 . . H H9B 0.728571 0.642875 0.071494 0.099 Uiso calc 1 . . C C10 0.8101(3) 0.5697(2) 0.1745(2) 0.0862(11) Uani d 1 . . H H10A 0.806032 0.516612 0.144085 0.103 Uiso calc 1 . . H H10B 0.895437 0.593736 0.180485 0.103 Uiso calc 1 . . C C11 0.8793(2) 0.49967(17) 0.3089(2) 0.0787(10) Uani d 1 . . H H11A 0.966542 0.520764 0.315213 0.094 Uiso calc 1 . . H H11B 0.873113 0.444775 0.281755 0.094 Uiso calc 1 . . C C12 0.8523(3) 0.49229(17) 0.3934(2) 0.0764(9) Uani d 1 . . H H12A 0.916935 0.456762 0.430318 0.092 Uiso calc 1 . . H H12B 0.855833 0.547403 0.419779 0.092 Uiso calc 1 . . O O1 0.72651(16) 0.45650(11) 0.38343(11) 0.0599(4) Uani d 1 . . O O2 0.46678(18) 0.44170(10) 0.39333(11) 0.0599(4) Uani d 1 . . O O3 0.27353(16) 0.46031(12) 0.23567(12) 0.0617(5) Uani d 1 . . O O4 0.32106(16) 0.56757(10) 0.11050(10) 0.0548(4) Uani d 1 . . O O5 0.58718(18) 0.58719(11) 0.10983(11) 0.0622(5) Uani d 1 . . O O6 0.78817(16) 0.55595(11) 0.25651(13) 0.0635(5) Uani d 1 . . C C13 0.51858(12) 0.64534(6) 0.29784(9) 0.0384(4) Uani d 1 . . C C14 0.63153(10) 0.68607(9) 0.34104(10) 0.0539(6) Uani d 1 . . H H14 0.709133 0.656479 0.356563 0.065 Uiso calc 1 . . C C15 0.62849(11) 0.77103(9) 0.36105(11) 0.0629(7) Uani d 1 . . H H15 0.704058 0.798278 0.389955 0.075 Uiso calc 1 . . C C16 0.51250(14) 0.81525(6) 0.33786(11) 0.0499(5) Uani d 1 . . C C17 0.39955(11) 0.77452(8) 0.29466(10) 0.0468(5) Uani d 1 . . C C18 0.40259(10) 0.68956(8) 0.27465(9) 0.0462(5) Uani d 1 . . H H18 0.327015 0.662312 0.245744 0.055 Uiso calc 1 . . F F1 0.50704(16) 0.89686(9) 0.35438(11) 0.0716(4) Uani d 1 . . F F2 0.29136(15) 0.81831(10) 0.27317(11) 0.0744(5) Uani d 1 . . N N1 0.52271(17) 0.55879(10) 0.27099(11) 0.0408(4) Uani d 1 . . H H1C 0.464130 0.550988 0.221364 0.049 Uiso calc 1 . . H H1D 0.505335 0.524893 0.310655 0.049 Uiso calc 1 . . H H1E 0.601222 0.547193 0.264402 0.049 Uiso calc 1 . . C C19 -0.0209(4) 0.7830(2) 0.3091(2) 0.1000(13) Uani d 1 . . H H19A -0.096678 0.751733 0.280924 0.150 Uiso calc 1 . . H H19B 0.022656 0.802363 0.267346 0.150 Uiso calc 1 . . H H19C -0.045808 0.830450 0.338254 0.150 Uiso calc 1 . . C C20 0.1128(3) 0.75246(17) 0.59978(17) 0.0601(6) Uani d 1 . . H H20A 0.148384 0.698150 0.618497 0.090 Uiso calc 1 . . H H20B 0.094406 0.781999 0.647350 0.090 Uiso calc 1 . . H H20C 0.174192 0.784069 0.577893 0.090 Uiso calc 1 . . N N2 0.00151(19) 0.68318(12) 0.44555(12) 0.0506(5) Uani d 1 . . O O7 0.1122(2) 0.64867(12) 0.33488(13) 0.0739(5) Uani d 1 . . O O8 0.1931(2) 0.76599(16) 0.42824(15) 0.0987(8) Uani d 1 . . O O9 -0.0738(2) 0.82343(12) 0.48981(12) 0.0719(5) Uani d 1 . . O O10 -0.1170(2) 0.69175(16) 0.55502(15) 0.0878(7) Uani d 1 . . S S1 0.08321(6) 0.71822(4) 0.38370(4) 0.05201(18) Uani d 1 . . S S2 -0.03064(6) 0.73997(4) 0.51857(4) 0.05091(18) Uani d 1 . . 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 0.087(2) 0.078(2) 0.0539(16) 0.0256(17) -0.0039(15) 0.0029(14) C2 0.106(2) 0.0697(19) 0.0691(18) 0.0251(18) 0.0318(18) 0.0272(15) C3 0.093(2) 0.0525(15) 0.0799(19) -0.0170(15) 0.0471(17) -0.0044(14) C4 0.0602(16) 0.0712(18) 0.088(2) -0.0189(14) 0.0405(15) -0.0192(15) C5 0.0385(13) 0.0548(15) 0.107(2) -0.0018(11) 0.0078(14) -0.0138(15) C6 0.0585(16) 0.0539(15) 0.0782(18) 0.0053(13) -0.0188(14) -0.0167(14) C7 0.092(2) 0.0682(17) 0.0420(13) 0.0320(16) 0.0039(13) 0.0005(12) C8 0.123(3) 0.0558(16) 0.0611(17) 0.0179(17) 0.0436(18) 0.0165(13) C9 0.099(2) 0.080(2) 0.085(2) -0.0323(19) 0.0529(19) -0.0086(17) C10 0.0682(19) 0.098(2) 0.109(3) -0.0248(18) 0.0546(19) -0.035(2) C11 0.0357(13) 0.0513(15) 0.148(3) 0.0017(12) 0.0202(16) -0.0165(18) C12 0.0464(14) 0.0475(15) 0.113(3) 0.0016(12) -0.0203(16) -0.0081(15) O1 0.0493(9) 0.0597(10) 0.0617(10) 0.0008(8) -0.0024(8) -0.0071(8) O2 0.0682(11) 0.0503(9) 0.0644(10) 0.0029(8) 0.0228(9) 0.0099(8) O3 0.0458(9) 0.0657(11) 0.0766(12) 0.0012(8) 0.0211(9) -0.0058(9) O4 0.0579(10) 0.0521(9) 0.0483(9) 0.0075(8) 0.0018(8) -0.0084(7) O5 0.0753(12) 0.0527(10) 0.0644(11) -0.0064(9) 0.0281(9) 0.0018(8) O6 0.0442(9) 0.0623(11) 0.0879(13) 0.0006(8) 0.0240(9) -0.0155(10) C13 0.0413(11) 0.0363(10) 0.0385(10) 0.0000(9) 0.0120(9) -0.0012(8) C14 0.0391(12) 0.0489(13) 0.0694(15) 0.0017(10) 0.0060(11) -0.0147(12) C15 0.0493(14) 0.0548(15) 0.0818(18) -0.0091(12) 0.0113(13) -0.0254(13) C16 0.0610(15) 0.0391(12) 0.0524(13) -0.0009(11) 0.0196(11) -0.0085(10) C17 0.0499(13) 0.0433(12) 0.0462(12) 0.0105(10) 0.0104(10) 0.0016(10) C18 0.0409(12) 0.0431(12) 0.0506(12) 0.0002(9) 0.0042(10) -0.0043(10) F1 0.0879(11) 0.0404(7) 0.0910(11) -0.0021(7) 0.0311(9) -0.0175(7) F2 0.0639(9) 0.0608(9) 0.0890(11) 0.0237(8) 0.0015(8) -0.0031(8) N1 0.0399(9) 0.0361(9) 0.0456(10) -0.0009(7) 0.0089(8) 0.0003(7) C19 0.142(3) 0.091(2) 0.077(2) 0.055(2) 0.047(2) 0.0332(19) C20 0.0613(16) 0.0622(16) 0.0529(14) -0.0056(13) 0.0071(12) -0.0050(12) N2 0.0535(11) 0.0411(10) 0.0551(11) -0.0075(9) 0.0101(9) -0.0032(9) O7 0.0820(13) 0.0653(12) 0.0791(13) 0.0081(10) 0.0293(11) -0.0180(10) O8 0.0957(16) 0.126(2) 0.0843(15) -0.0665(15) 0.0405(13) -0.0407(14) O9 0.0779(13) 0.0623(12) 0.0745(12) 0.0270(10) 0.0171(10) 0.0010(9) O10 0.0747(14) 0.1093(17) 0.0896(14) -0.0358(13) 0.0399(12) -0.0029(13) S1 0.0551(4) 0.0459(3) 0.0557(3) -0.0069(3) 0.0152(3) -0.0079(3) S2 0.0439(3) 0.0534(3) 0.0556(3) -0.0043(2) 0.0129(3) 0.0001(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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l 0 0 1 0 0 -1 0 0 -1 0 0 -1 0 0 1 0 0 -2 0 0 2 0 0 -2 0 0 -2 0 0 2 0 0 2 0 0 3 0 0 -3 0 0 -3 0 0 3 0 0 3 0 0 -3 0 0 -4 0 0 -4 0 0 4 0 0 4 0 0 -4 0 0 4 0 0 4 0 0 5 0 0 -5 0 0 5 0 0 5 0 0 5 0 0 -5 0 0 -6 0 0 -6 0 0 6 0 0 6 0 0 6 0 0 7 0 0 7 0 0 7 0 0 -7 0 0 7 0 0 7 0 0 8 0 0 8 0 0 8 0 0 8 0 0 8 0 0 9 0 0 9 0 0 9 0 0 9 0 0 10 0 0 10 0 0 10 0 0 10 0 0 10 0 0 11 0 0 11 0 0 11 0 0 -11 0 0 12 0 0 12 0 0 12 0 0 -12 0 0 13 0 0 13 0 0 13 0 0 -13 0 0 -14 0 0 14 0 0 14 0 0 15 0 0 15 0 0 -15 0 0 -15 0 0 15 0 0 16 0 0 16 0 0 16 0 0 -16 0 0 17 0 0 17 0 0 -17 0 0 18 0 0 18 0 0 -18 0 0 18 0 1 0 0 -1 0 0 1 -1 0 -1 1 0 1 1 0 -1 1 0 1 -1 0 -1 -1 0 1 1 0 -1 -1 0 -1 1 0 1 -1 0 -1 -1 0 1 1 0 1 1 0 1 -1 0 -1 -2 0 -1 2 0 1 2 0 1 2 0 -1 2 0 1 2 0 -1 -2 0 1 2 0 1 -2 0 -1 2 0 1 2 0 -1 2 0 1 -3 0 1 3 0 -1 3 0 -1 3 0 1 3 0 -1 3 0 1 3 0 1 3 0 1 3 0 1 3 0 -1 3 0 -1 -3 0 -1 4 0 1 -4 0 1 4 0 1 4 0 -1 4 0 -1 -4 0 1 4 0 1 -4 0 -1 4 0 1 4 0 1 4 0 1 4 0 1 -5 0 -1 5 0 1 5 0 -1 -5 0 1 5 0 -1 -5 0 -1 -5 0 1 5 0 -1 5 0 1 5 0 1 5 0 -1 5 0 1 5 0 1 6 0 1 6 0 1 6 0 -1 6 0 1 6 0 1 -6 0 -1 -6 0 -1 -6 0 -1 7 0 1 7 0 1 7 0 -1 7 0 1 7 0 -1 7 0 -1 -7 0 1 7 0 1 7 0 -1 7 0 1 8 0 -1 8 0 -1 -8 0 -1 8 0 -1 8 0 1 8 0 -1 8 0 1 8 0 -1 8 0 -1 -8 0 1 8 0 -1 -9 0 1 -9 0 1 9 0 -1 9 0 -1 9 0 -1 9 0 -1 9 0 -1 9 0 1 9 0 1 -10 0 1 10 0 -1 10 0 1 10 0 -1 10 0 -1 10 0 1 10 0 1 10 0 1 -11 0 -1 11 0 1 11 0 -1 11 0 1 11 0 -1 11 0 -1 11 0 1 11 0 1 11 0 -1 11 0 -1 -12 0 1 -12 0 -1 12 0 1 12 0 -1 12 0 1 12 0 1 12 0 -1 12 0 -1 13 0 1 13 0 -1 13 0 1 -13 0 -1 -13 0 -1 13 0 1 13 0 1 13 0 1 -13 0 1 -14 0 -1 -14 0 -1 14 0 1 14 0 -1 14 0 1 14 0 1 -14 0 1 15 0 1 15 0 -1 15 0 1 -15 0 -1 15 0 1 15 0 -1 15 0 1 -15 0 -1 -15 0 -1 16 0 1 16 0 -1 16 0 1 16 0 -1 -16 0 1 -16 0 -1 16 0 1 17 0 -1 17 0 1 17 0 -1 17 0 -1 -17 0 1 -17 0 -1 17 0 -1 18 0 -1 -18 0 1 -18 0 1 18 0 -1 18 0 1 18 0 -2 0 0 2 0 0 2 1 0 2 -1 0 2 1 0 2 1 0 -2 -1 0 2 -1 0 -2 -1 0 -2 1 0 2 2 0 2 2 0 2 -2 0 2 2 0 -2 2 0 2 2 0 2 2 0 2 2 0 2 -2 0 2 2 0 -2 2 0 2 -2 0 -2 -2 0 2 3 0 2 3 0 2 -3 0 2 3 0 -2 3 0 2 -3 0 -2 3 0 2 3 0 2 3 0 -2 -3 0 -2 -3 0 2 3 0 2 4 0 2 4 0 2 -4 0 -2 4 0 -2 4 0 -2 -4 0 2 4 0 2 4 0 -2 4 0 2 4 0 -2 -4 0 2 -4 0 2 4 0 2 4 0 2 5 0 -2 5 0 -2 5 0 2 -5 0 2 5 0 2 5 0 2 5 0 -2 5 0 2 5 0 -2 -5 0 2 -5 0 2 5 0 2 -6 0 -2 -6 0 -2 6 0 2 6 0 -2 -6 0 -2 -6 0 2 6 0 2 6 0 2 6 0 -2 7 0 2 7 0 -2 -7 0 2 7 0 -2 7 0 2 -7 0 2 7 0 2 7 0 -2 -8 0 2 -8 0 -2 8 0 2 8 0 2 8 0 -2 8 0 -2 8 0 2 9 0 -2 9 0 -2 -9 0 -2 9 0 2 9 0 -2 9 0 -2 -9 0 2 -9 0 -2 9 0 2 9 0 2 10 0 -2 -10 0 2 -10 0 2 10 0 -2 -10 0 -2 10 0 -2 10 0 2 10 0 2 10 0 -2 10 0 2 -11 0 2 -11 0 -2 11 0 2 11 0 2 11 0 -2 11 0 -2 11 0 -2 11 0 2 11 0 -2 11 0 2 11 0 2 12 0 -2 12 0 2 -12 0 2 -12 0 2 12 0 -2 12 0 -2 12 0 2 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0 4 8 0 -4 -8 0 4 -8 0 4 8 0 -4 9 0 4 -9 0 -4 -9 0 -4 9 0 -4 -9 0 4 9 0 4 9 0 4 -9 0 4 9 0 4 10 0 4 10 0 -4 10 0 4 10 0 4 -10 0 -4 -10 0 4 10 0 4 -10 0 -4 -10 0 -4 10 0 -4 10 0 -4 11 0 -4 11 0 -4 11 0 4 -11 0 4 11 0 4 -11 0 -4 11 0 4 11 0 -4 11 0 4 11 0 -4 -11 0 -4 12 0 -4 12 0 4 12 0 4 -12 0 -4 12 0 -4 12 0 -4 12 0 4 12 0 4 13 0 -4 13 0 -4 13 0 -4 13 0 4 -13 0 -4 14 0 4 14 0 -4 14 0 -4 14 0 4 -14 0 -4 15 0 -4 15 0 -4 16 0 4 16 0 4 -16 0 -4 16 0 -4 16 0 -4 17 0 -4 -17 0 4 -17 0 -4 17 0 -4 17 0 4 17 0 -4 -18 0 -4 18 0 4 18 0 5 0 0 5 0 0 -5 0 0 5 0 0 -5 1 0 5 -1 0 5 1 0 5 -1 0 5 1 0 5 -1 0 5 1 0 5 -1 0 5 -2 0 5 2 0 -5 -2 0 5 -2 0 5 2 0 5 2 0 5 -2 0 5 2 0 -5 -2 0 -5 3 0 -5 -3 0 -5 3 0 5 3 0 5 -3 0 5 3 0 5 -3 0 5 -3 0 5 3 0 -5 3 0 -5 -4 0 -5 -4 0 -5 4 0 5 4 0 5 -4 0 5 4 0 5 -4 0 5 4 0 5 -5 0 5 5 0 5 5 0 -5 -5 0 5 5 0 5 -5 0 -5 5 0 5 5 0 5 5 0 -5 -5 0 -5 5 0 -5 -6 0 5 6 0 5 6 0 5 6 0 5 -6 0 5 -6 0 5 6 0 -5 6 0 -5 6 0 -5 7 0 5 7 0 5 7 0 5 7 0 -5 7 0 5 -7 0 -5 -8 0 5 8 0 5 8 0 -5 8 0 -5 8 0 5 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10 6 -11 10 6 11 -10 -6 11 -10 -5 -11 10 5 11 -10 -4 -11 10 4 11 -10 -3 -11 10 3 11 -10 -2 -11 10 2 11 -10 -1 -11 10 1 12 0 -12 12 0 -11 12 0 -10 12 0 -9 12 0 -9 12 0 -8 12 0 -8 12 0 -8 12 0 -7 12 0 -7 12 0 -7 12 0 -6 12 0 -6 12 0 -6 12 0 -5 12 0 -5 12 0 -4 12 0 -3 12 0 -2 12 0 -2 12 0 -2 12 0 -1 12 0 -1 12 0 -1 12 0 0 12 0 0 12 0 1 12 0 1 12 0 2 12 0 2 12 0 3 12 0 3 12 1 -12 12 -1 -12 12 1 -11 12 -1 -11 12 1 -10 12 -1 -10 12 -1 -9 12 -1 -9 12 1 -9 12 -1 -9 12 -1 -8 12 -1 -8 12 1 -8 12 1 -8 12 -1 -8 12 1 -7 12 -1 -7 12 -1 -7 12 1 -7 12 -1 -7 12 1 -6 12 -1 -6 12 -1 -6 12 1 -6 12 -1 -6 12 -1 -5 12 1 -5 12 -1 -5 12 1 -5 12 -1 -5 12 -1 -4 12 1 -4 12 1 -3 12 1 -3 12 -1 -3 12 1 -3 12 -1 -2 12 1 -2 12 -1 -2 12 1 -2 12 -1 -2 12 1 -2 12 -1 -1 12 1 -1 12 -1 -1 12 -1 -1 12 1 -1 12 -1 0 12 1 0 12 -1 0 12 1 0 12 -1 1 12 1 1 12 -1 1 12 1 1 12 -1 2 12 1 2 12 -1 2 12 1 2 12 -1 3 12 1 3 12 -1 3 12 1 3 12 2 -11 12 -2 -11 12 2 -10 12 -2 -10 12 -2 -9 12 -2 -9 12 2 -9 12 -2 -9 12 -2 -8 12 -2 -8 12 -2 -8 12 2 -8 12 2 -7 12 -2 -7 12 2 -7 12 -2 -7 12 -2 -7 12 2 -6 12 -2 -6 12 2 -6 12 -2 -6 12 -2 -6 12 2 -5 12 -2 -5 12 -2 -5 12 2 -5 12 -2 -5 12 2 -4 12 -2 -4 12 2 -3 12 2 -3 12 -2 -3 12 2 -3 12 2 -2 12 -2 -2 12 2 -2 12 -2 -1 12 2 -1 12 -2 -1 12 -2 -1 12 2 -1 12 -2 0 12 2 0 12 -2 0 12 2 0 12 -2 1 12 2 1 12 -2 1 12 2 1 12 -2 2 12 2 2 12 -2 2 12 2 2 12 -2 3 12 2 3 12 -2 3 12 2 3 12 -3 -11 12 3 -10 12 -3 -10 12 -3 -9 12 3 -9 12 -3 -9 12 -3 -8 12 -3 -8 12 3 -8 12 -3 -8 12 -3 -7 12 -3 -7 12 3 -7 12 -3 -7 12 -3 -6 12 -3 -6 12 3 -6 12 -3 -6 12 -3 -5 12 -3 -5 12 -3 -5 12 -3 -4 12 3 -4 12 3 -3 12 -3 -3 12 3 -3 12 3 -2 12 -3 -2 12 3 -2 12 3 -1 12 -3 -1 12 3 -1 12 3 0 12 -3 0 12 -3 0 12 -3 0 12 3 0 12 3 1 12 -3 1 12 -3 1 12 3 1 12 -3 2 12 3 2 12 3 2 12 -3 2 12 -4 -11 12 -4 -10 12 -4 -9 12 -4 -9 12 -4 -8 12 -4 -8 12 -4 -7 12 -4 -7 12 -4 -7 12 -4 -6 12 -4 -6 12 -4 -6 12 -4 -5 12 -4 -5 12 -4 -4 12 -4 -3 12 4 -2 12 -4 -2 12 4 -1 12 -4 -1 12 4 0 12 -4 0 12 4 1 12 -4 1 12 -4 1 12 -4 2 12 -5 -10 12 -5 -9 12 -5 -8 12 -5 -8 12 -5 -7 12 -5 -7 12 -5 -6 12 -5 -6 12 -5 -5 12 -5 -5 12 -5 -4 12 -5 -3 12 -5 -2 12 -5 -1 12 -5 0 12 -6 -9 12 -6 -8 12 -6 -8 12 -6 -7 12 -6 -7 12 -6 -6 12 -6 -6 12 -6 -5 12 -6 -4 12 -6 -3 12 -6 -2 12 -6 -1 12 -6 0 12 -7 -8 12 -7 -7 12 -7 -6 12 -7 -6 12 -7 -5 12 -7 -4 12 -7 -3 12 -7 -2 12 -7 -1 13 0 -5 13 0 -4 13 -1 -6 13 -1 -5 13 -1 -4 13 -2 -7 13 -2 -6 13 -2 -5 13 -2 -4 13 -3 -5 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 H1A C1 H1B . . 108.3 ? C2 C1 H1A . . 109.9 ? C2 C1 H1B . . 109.9 ? O1 C1 H1A . . 109.9 ? O1 C1 H1B . . 109.9 ? O1 C1 C2 . . 108.8(2) ? C1 C2 H2A . . 109.7 ? C1 C2 H2B . . 109.7 ? H2A C2 H2B . . 108.2 ? O2 C2 C1 . . 109.7(2) ? O2 C2 H2A . . 109.7 ? O2 C2 H2B . . 109.7 ? H3A C3 H3B . . 108.2 ? C4 C3 H3A . . 109.7 ? C4 C3 H3B . . 109.7 ? O2 C3 H3A . . 109.7 ? O2 C3 H3B . . 109.7 ? O2 C3 C4 . . 109.7(2) ? C3 C4 H4A . . 110.0 ? C3 C4 H4B . . 110.0 ? H4A C4 H4B . . 108.3 ? O3 C4 C3 . . 108.7(2) ? O3 C4 H4A . . 110.0 ? O3 C4 H4B . . 110.0 ? H5A C5 H5B . . 108.3 ? C6 C5 H5A . . 109.9 ? C6 C5 H5B . . 109.9 ? O3 C5 H5A . . 109.9 ? O3 C5 H5B . . 110.0 ? O3 C5 C6 . . 108.7(2) ? C5 C6 H6A . . 109.9 ? C5 C6 H6B . . 109.9 ? H6A C6 H6B . . 108.3 ? O4 C6 C5 . . 109.1(2) ? O4 C6 H6A . . 109.9 ? O4 C6 H6B . . 109.9 ? H7A C7 H7B . . 108.3 ? C8 C7 H7A . . 110.0 ? C8 C7 H7B . . 110.0 ? O4 C7 H7A . . 110.0 ? O4 C7 H7B . . 110.0 ? O4 C7 C8 . . 108.7(2) ? C7 C8 H8A . . 109.9 ? C7 C8 H8B . . 109.9 ? H8A C8 H8B . . 108.3 ? O5 C8 C7 . . 109.1(2) ? O5 C8 H8A . . 109.9 ? O5 C8 H8B . . 109.9 ? H9A C9 H9B . . 108.4 ? C10 C9 H9A . . 110.0 ? C10 C9 H9B . . 110.0 ? O5 C9 H9A . . 110.0 ? O5 C9 H9B . . 110.0 ? O5 C9 C10 . . 108.5(2) ? C9 C10 H10A . . 109.9 ? C9 C10 H10B . . 109.9 ? H10A C10 H10B . . 108.3 ? O6 C10 C9 . . 108.9(2) ? O6 C10 H10A . . 109.9 ? O6 C10 H10B . . 109.9 ? H11A C11 H11B . . 108.2 ? C12 C11 H11A . . 109.8 ? C12 C11 H11B . . 109.8 ? O6 C11 H11A . . 109.8 ? O6 C11 H11B . . 109.8 ? O6 C11 C12 . . 109.5(2) ? C11 C12 H12A . . 109.9 ? C11 C12 H12B . . 109.9 ? H12A C12 H12B . . 108.3 ? O1 C12 C11 . . 109.1(2) ? O1 C12 H12A . . 109.9 ? O1 C12 H12B . . 109.9 ? C1 O1 C12 . . 112.9(2) ? C3 O2 C2 . . 113.2(2) ? C5 O3 C4 . . 113.3(2) ? C7 O4 C6 . . 113.3(2) ? C8 O5 C9 . . 113.9(2) ? C10 O6 C11 . . 113.5(2) ? C14 C13 C18 . . 120.0 ? C14 C13 N1 . . 120.29(11) ? C18 C13 N1 . . 119.54(11) ? C13 C14 H14 . . 120.0 ? C13 C14 C15 . . 120.0 ? C15 C14 H14 . . 120.0 ? C14 C15 H15 . . 120.0 ? C14 C15 C16 . . 120.0 ? C16 C15 H15 . . 120.0 ? C17 C16 C15 . . 120.0 ? F1 C16 C15 . . 121.40(12) ? F1 C16 C17 . . 118.59(12) ? C18 C17 C16 . . 120.0 ? F2 C17 C16 . . 118.51(12) ? F2 C17 C18 . . 121.48(12) ? C13 C18 H18 . . 120.0 ? C17 C18 C13 . . 120.0 ? C17 C18 H18 . . 120.0 ? C13 N1 H1C . . 109.5 ? C13 N1 H1D . . 109.5 ? C13 N1 H1E . . 109.5 ? H1C N1 H1D . . 109.5 ? H1C N1 H1E . . 109.5 ? H1D N1 H1E . . 109.5 ? H19A C19 H19B . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? S1 C19 H19A . . 109.5 ? S1 C19 H19B . . 109.5 ? S1 C19 H19C . . 109.5 ? H20A C20 H20B . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? S2 C20 H20A . . 109.5 ? S2 C20 H20B . . 109.5 ? S2 C20 H20C . . 109.5 ? S1 N2 S2 . . 121.55(12) ? N2 S1 C19 . . 106.47(15) ? O7 S1 C19 . . 105.36(15) ? O7 S1 N2 . . 107.66(11) ? O8 S1 C19 . . 109.29(19) ? O8 S1 N2 . . 112.58(12) ? O8 S1 O7 . . 114.93(14) ? N2 S2 C20 . . 107.74(12) ? O9 S2 C20 . . 106.46(13) ? O9 S2 N2 . . 113.37(11) ? O10 S2 C20 . . 106.61(14) ? O10 S2 N2 . . 106.33(13) ? O10 S2 O9 . . 115.88(14) ? 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 H1A . 0.9700 ? C1 H1B . 0.9700 ? C1 C2 . 1.476(5) ? C1 O1 . 1.411(3) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C2 O2 . 1.426(3) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C3 C4 . 1.471(4) ? C3 O2 . 1.424(3) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C4 O3 . 1.426(3) ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C5 C6 . 1.477(4) ? C5 O3 . 1.414(3) ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? C6 O4 . 1.426(3) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C7 C8 . 1.480(4) ? C7 O4 . 1.426(3) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C8 O5 . 1.421(3) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C9 C10 . 1.485(5) ? C9 O5 . 1.423(3) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C10 O6 . 1.415(4) ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C11 C12 . 1.465(5) ? C11 O6 . 1.429(3) ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ? C12 O1 . 1.429(3) ? C13 C14 . 1.3900 ? C13 C18 . 1.3900 ? C13 N1 . 1.4455(19) ? C14 H14 . 0.9300 ? C14 C15 . 1.3900 ? C15 H15 . 0.9300 ? C15 C16 . 1.3900 ? C16 C17 . 1.3900 ? C16 F1 . 1.3279(16) ? C17 C18 . 1.3900 ? C17 F2 . 1.3172(17) ? C18 H18 . 0.9300 ? N1 H1C . 0.8900 ? N1 H1D . 0.8900 ? N1 H1E . 0.8900 ? C19 H19A . 0.9600 ? C19 H19B . 0.9600 ? C19 H19C . 0.9600 ? C19 S1 . 1.750(3) ? C20 H20A . 0.9600 ? C20 H20B . 0.9600 ? C20 H20C . 0.9600 ? C20 S2 . 1.756(3) ? N2 S1 . 1.581(2) ? N2 S2 . 1.587(2) ? O7 S1 . 1.4341(19) ? O8 S1 . 1.428(2) ? O9 S2 . 1.4412(19) ? O10 S2 . 1.433(2) ? 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 N1 H1C O4 . 0.89 2.05 2.918(2) 164.3 yes N1 H1D O2 . 0.89 1.99 2.879(2) 175.6 yes N1 H1E O6 . 0.89 2.04 2.901(2) 163.8 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 C1 C2 O2 C3 . . . . 173.5(2) ? C2 C1 O1 C12 . . . . -169.5(2) ? C3 C4 O3 C5 . . . . 174.6(2) ? C4 C3 O2 C2 . . . . 177.3(2) ? C5 C6 O4 C7 . . . . 179.0(2) ? C6 C5 O3 C4 . . . . -178.7(2) ? C7 C8 O5 C9 . . . . 171.3(2) ? C8 C7 O4 C6 . . . . -178.5(2) ? C9 C10 O6 C11 . . . . 179.4(2) ? C10 C9 O5 C8 . . . . -176.4(2) ? C11 C12 O1 C1 . . . . -178.6(2) ? C12 C11 O6 C10 . . . . 177.6(2) ? O1 C1 C2 O2 . . . . -66.8(3) ? O2 C3 C4 O3 . . . . 69.3(3) ? O3 C5 C6 O4 . . . . -63.4(3) ? O4 C7 C8 O5 . . . . 70.4(3) ? O5 C9 C10 O6 . . . . -65.7(3) ? O6 C11 C12 O1 . . . . 62.8(3) ? C13 C14 C15 C16 . . . . 0.0 ? C14 C13 C18 C17 . . . . 0.0 ? C14 C15 C16 C17 . . . . 0.0 ? C14 C15 C16 F1 . . . . -178.49(17) ? C15 C16 C17 C18 . . . . 0.0 ? C15 C16 C17 F2 . . . . -179.64(16) ? C16 C17 C18 C13 . . . . 0.0 ? C18 C13 C14 C15 . . . . 0.0 ? F1 C16 C17 C18 . . . . 178.53(16) ? F1 C16 C17 F2 . . . . -1.11(18) ? F2 C17 C18 C13 . . . . 179.63(17) ? N1 C13 C14 C15 . . . . 175.22(15) ? N1 C13 C18 C17 . . . . -175.25(15) ? S1 N2 S2 C20 . . . . -72.33(17) ? S1 N2 S2 O9 . . . . 45.21(19) ? S1 N2 S2 O10 . . . . 173.68(15) ? S2 N2 S1 C19 . . . . -76.3(2) ? S2 N2 S1 O7 . . . . 171.11(14) ? S2 N2 S1 O8 . . . . 43.4(2) ? _cod_database_fobs_code 2312735