#------------------------------------------------------------------------------ #$Date: 2024-12-18 05:01:29 +0200 (Wed, 18 Dec 2024) $ #$Revision: 296910 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312736.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_2312736 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 104.4828(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.57046(14) _cell_length_b 15.7746(2) _cell_length_c 15.8622(2) _cell_measurement_reflns_used 16092 _cell_measurement_temperature 100.0(3) _cell_measurement_theta_max 71.9860 _cell_measurement_theta_min 3.9710 _cell_volume 2560.89(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 100.0(3) _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 0.982 _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 0.0320 _diffrn_reflns_av_unetI/netI 0.0259 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 26263 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.996 _diffrn_reflns_theta_min 4.017 _diffrn_source 'Rotating-anode X-ray tube' _exptl_absorpt_coefficient_mu 2.522 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis PRO; Rigaku OD, 2024) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.470 _exptl_crystal_description block _exptl_crystal_F_000 1200 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.451 _refine_diff_density_min -0.474 _refine_ls_extinction_coef 0.00024(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 329 _refine_ls_number_reflns 4949 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0324 _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^)+(0.0396P)^2^+1.1759P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.0846 _reflns_number_gt 4247 _reflns_number_total 4949 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL zy_240926_1_100k_auto_a.res in P2(1)/c zy_240926_1_100k_auto.res created by SHELXL-2018/3 at 11:33:14 on 10-Oct-2024 REM Old TITL zy_240926_1_100k_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.109, Rweak 0.008, Alpha 0.028 REM 0.376 for 96 systematic absences, Orientation as input REM Formula found by SHELXT: C7 N1 N1 F2 S2 CELL 1.54184 10.57046 15.7746 15.862167 90 104.4828 90 ZERR 4 0.000136 0.000211 0.000219 0 0.0014 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. 30 PLAN 3 SIZE 0.08 0.07 0.06 TEMP -173 CONF HTAB N1 O1 HTAB N1 O5 HTAB N1 O3 BOND fmap 2 acta MORE -1 BOND $H REM REM REM WGHT 0.039600 1.175900 EXTI 0.000242 FVAR 3.39569 S1 6 1.085420 0.284130 0.379583 11.00000 0.02454 0.02001 = 0.02371 0.00348 0.00752 0.00381 S2 6 0.973263 0.260131 0.517999 11.00000 0.01846 0.02154 = 0.02300 -0.00034 0.00544 0.00144 F1 3 0.511993 0.100543 0.354167 11.00000 0.03403 0.01794 = 0.03587 0.00550 0.01155 0.00033 F2 3 0.292418 0.179724 0.273604 11.00000 0.02450 0.02505 = 0.03134 0.00012 0.00272 -0.00798 O1 5 0.321817 0.433325 0.109634 11.00000 0.02454 0.02242 = 0.02068 0.00261 0.00368 -0.00026 O2 5 0.589782 0.411347 0.106331 11.00000 0.02890 0.02210 = 0.02963 -0.00073 0.01044 0.00220 O3 5 0.791311 0.444718 0.254253 11.00000 0.02078 0.02737 = 0.03569 0.00379 0.01026 -0.00177 O4 5 0.732444 0.547129 0.383916 11.00000 0.02081 0.02620 = 0.02743 0.00344 -0.00012 0.00150 O5 5 0.469249 0.558338 0.395228 11.00000 0.02587 0.02185 = 0.02632 -0.00348 0.00655 -0.00109 O6 5 0.271311 0.544636 0.233929 11.00000 0.02162 0.02885 = 0.02853 -0.00126 0.00894 -0.00343 O7 5 1.114177 0.355285 0.330176 11.00000 0.03262 0.02581 = 0.03033 0.00579 0.00973 -0.00337 O8 5 1.197343 0.234907 0.424151 11.00000 0.03883 0.05106 = 0.03547 0.01612 0.01756 0.02511 O9 5 0.930292 0.175537 0.487761 11.00000 0.02887 0.02396 = 0.02886 -0.00055 0.00726 -0.00675 O10 5 0.885680 0.307428 0.556963 11.00000 0.02743 0.03926 = 0.03371 -0.00144 0.01263 0.00975 N1 4 0.524230 0.442346 0.270310 11.00000 0.01917 0.01713 = 0.02060 -0.00057 0.00376 0.00023 AFIX 137 H1C 2 0.461319 0.451336 0.220282 11.00000 -1.20000 H1D 2 0.603943 0.454620 0.261303 11.00000 -1.20000 H1E 2 0.509198 0.476322 0.313143 11.00000 -1.20000 AFIX 0 N2 4 1.003170 0.319089 0.443613 11.00000 0.02390 0.01730 = 0.02395 0.00091 0.00543 0.00375 C1 1 0.365302 0.417201 0.032334 11.00000 0.03529 0.02599 = 0.01938 -0.00054 0.00542 -0.00970 AFIX 23 H1A 2 0.386452 0.471272 0.007264 11.00000 -1.20000 H1B 2 0.295614 0.388345 -0.011684 11.00000 -1.20000 AFIX 0 C2 1 0.484111 0.362217 0.056483 11.00000 0.04343 0.02185 = 0.02654 -0.00577 0.01595 -0.00568 AFIX 23 H2A 2 0.467461 0.313087 0.091029 11.00000 -1.20000 H2B 2 0.506046 0.340649 0.003262 11.00000 -1.20000 AFIX 0 C3 1 0.712224 0.368468 0.122582 11.00000 0.03712 0.03114 = 0.03543 0.00338 0.01915 0.01220 AFIX 23 H3A 2 0.731332 0.351745 0.066887 11.00000 -1.20000 H3B 2 0.709781 0.316629 0.157320 11.00000 -1.20000 AFIX 0 C4 1 0.815327 0.427559 0.171430 11.00000 0.02830 0.03754 = 0.04184 0.01203 0.01912 0.00791 AFIX 23 H4A 2 0.902653 0.401462 0.179119 11.00000 -1.20000 H4B 2 0.813402 0.481006 0.138420 11.00000 -1.20000 AFIX 0 C5 1 0.884337 0.502455 0.305309 11.00000 0.01607 0.02183 = 0.06065 0.00390 0.00845 -0.00109 AFIX 23 H5A 2 0.876221 0.558584 0.276532 11.00000 -1.20000 H5B 2 0.974082 0.481140 0.310625 11.00000 -1.20000 AFIX 0 C6 1 0.859482 0.510584 0.393119 11.00000 0.01954 0.02176 = 0.04612 0.00006 -0.00675 0.00200 AFIX 23 H6A 2 0.863463 0.454107 0.420879 11.00000 -1.20000 H6B 2 0.926849 0.547190 0.430437 11.00000 -1.20000 AFIX 0 C7 1 0.696664 0.549613 0.464547 11.00000 0.03384 0.02914 = 0.02393 0.00117 -0.00160 -0.00793 AFIX 23 H7A 2 0.768173 0.574885 0.510153 11.00000 -1.20000 H7B 2 0.680525 0.491440 0.482836 11.00000 -1.20000 AFIX 0 C8 1 0.575500 0.601866 0.452915 11.00000 0.04015 0.02891 = 0.02671 -0.00934 0.00959 -0.00967 AFIX 23 H8A 2 0.555432 0.611015 0.509943 11.00000 -1.20000 H8B 2 0.588645 0.657881 0.428267 11.00000 -1.20000 AFIX 0 C9 1 0.354671 0.610227 0.371378 11.00000 0.03363 0.02099 = 0.03169 0.00140 0.01640 0.00571 AFIX 23 H9A 2 0.371993 0.660247 0.338265 11.00000 -1.20000 H9B 2 0.330740 0.630519 0.424397 11.00000 -1.20000 AFIX 0 C10 1 0.244738 0.559370 0.316681 11.00000 0.02528 0.02772 = 0.03108 0.00558 0.01358 0.00559 AFIX 23 H10A 2 0.236833 0.504678 0.345546 11.00000 -1.20000 H10B 2 0.161409 0.590616 0.309041 11.00000 -1.20000 AFIX 0 C11 1 0.169106 0.498774 0.176027 11.00000 0.01692 0.02225 = 0.03868 0.00292 0.00350 0.00016 AFIX 23 H11A 2 0.086447 0.531239 0.165171 11.00000 -1.20000 H11B 2 0.155649 0.443498 0.202035 11.00000 -1.20000 AFIX 0 C12 1 0.207484 0.485229 0.092373 11.00000 0.02349 0.02278 = 0.02972 0.00452 -0.00336 -0.00119 AFIX 23 H12A 2 0.135557 0.457089 0.049429 11.00000 -1.20000 H12B 2 0.225535 0.540395 0.067996 11.00000 -1.20000 AFIX 0 C13 1 0.521368 0.353154 0.296472 11.00000 0.02124 0.01651 = 0.01749 -0.00001 0.00625 -0.00009 C14 1 0.635874 0.313207 0.339753 11.00000 0.01931 0.02354 = 0.02484 0.00223 0.00399 -0.00126 AFIX 43 H14 2 0.715431 0.344133 0.355477 11.00000 -1.20000 AFIX 0 C15 1 0.633693 0.227531 0.360062 11.00000 0.02156 0.02471 = 0.02999 0.00744 0.00561 0.00417 AFIX 43 H15 2 0.711454 0.199452 0.390045 11.00000 -1.20000 AFIX 0 C16 1 0.517750 0.184108 0.336220 11.00000 0.02958 0.01633 = 0.02290 0.00302 0.01017 0.00061 C17 1 0.403575 0.224924 0.295119 11.00000 0.01989 0.02165 = 0.01975 -0.00270 0.00524 -0.00466 C18 1 0.403179 0.309709 0.274597 11.00000 0.01905 0.02132 = 0.02177 0.00159 0.00364 0.00183 AFIX 43 H18 2 0.324460 0.337741 0.246310 11.00000 -1.20000 AFIX 0 C19 1 0.979853 0.218079 0.304401 11.00000 0.05648 0.03288 = 0.03010 -0.00877 0.01757 -0.01699 AFIX 137 H19A 2 0.903305 0.250644 0.273509 11.00000 -1.50000 H19B 2 0.951656 0.170727 0.335318 11.00000 -1.50000 H19C 2 1.025720 0.196027 0.262443 11.00000 -1.50000 AFIX 0 C20 1 1.120062 0.247395 0.599102 11.00000 0.02461 0.02493 = 0.02169 0.00147 0.00356 0.00153 AFIX 137 H20A 2 1.102755 0.215876 0.648274 11.00000 -1.50000 H20B 2 1.156054 0.303224 0.619071 11.00000 -1.50000 H20C 2 1.183023 0.216001 0.575068 11.00000 -1.50000 AFIX 0 HKLF 4 REM zy_240926_1_100k_auto_a.res in P2(1)/c REM wR2 = 0.0846, GooF = S = 1.046, Restrained GooF = 1.046 for all data REM R1 = 0.0324 for 4247 Fo > 4sig(Fo) and 0.0399 for all 4949 data REM 329 parameters refined using 0 restraints END WGHT 0.0396 1.1765 REM Highest difference peak 0.451, deepest hole -0.474, 1-sigma level 0.046 Q1 1 1.1348 0.1970 0.3992 11.00000 0.05 0.45 Q2 1 1.0245 0.2532 0.3423 11.00000 0.05 0.40 Q3 1 0.4672 0.3338 0.2922 11.00000 0.05 0.24 REM The information below was added by Olex2. REM REM R1 = 0.0324 for 4247 Fo > 4sig(Fo) and 0.0399 for all 27013 data REM 329 parameters refined using n/a restraints REM Highest difference peak 0.45, deepest hole -0.47 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0399 REM R1_gt = 0.0324 REM wR_ref = 0.0846 REM GOOF = 1.046 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 27013 REM Reflections_gt = 4247 REM Parameters = 329 REM Hole = -0.47 REM Peak = 0.45 REM Flack = n/a ; _cod_data_source_file dg3066sup1.cif _cod_data_source_block zy_240926_1_100k_auto _cod_original_cell_volume 2560.88(6) _cod_database_code 2312736 _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 0.824 _shelx_estimated_absorpt_t_max 0.863 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 S S1 1.08542(4) 0.28413(3) 0.37958(3) 0.02249(11) Uani d 1 . . S S2 0.97326(4) 0.26013(3) 0.51800(3) 0.02096(11) Uani d 1 . . F F1 0.51199(10) 0.10054(6) 0.35417(7) 0.0288(2) Uani d 1 . . F F2 0.29242(9) 0.17972(6) 0.27360(6) 0.0277(2) Uani d 1 . . O O1 0.32182(11) 0.43332(7) 0.10963(7) 0.0229(3) Uani d 1 . . O O2 0.58978(11) 0.41135(7) 0.10633(8) 0.0263(3) Uani d 1 . . O O3 0.79131(11) 0.44472(8) 0.25425(8) 0.0274(3) Uani d 1 . . O O4 0.73244(11) 0.54713(8) 0.38392(8) 0.0259(3) Uani d 1 . . O O5 0.46925(11) 0.55834(7) 0.39523(7) 0.0247(3) Uani d 1 . . O O6 0.27131(11) 0.54464(8) 0.23393(8) 0.0259(3) Uani d 1 . . O O7 1.11418(12) 0.35528(8) 0.33018(8) 0.0293(3) Uani d 1 . . O O8 1.19734(13) 0.23491(9) 0.42415(9) 0.0403(4) Uani d 1 . . O O9 0.93029(12) 0.17554(8) 0.48776(8) 0.0272(3) Uani d 1 . . O O10 0.88568(12) 0.30743(9) 0.55696(8) 0.0326(3) Uani d 1 . . N N1 0.52423(13) 0.44235(8) 0.27031(9) 0.0192(3) Uani d 1 . . H H1C 0.461319 0.451336 0.220282 0.023 Uiso calc 1 . . H H1D 0.603943 0.454620 0.261303 0.023 Uiso calc 1 . . H H1E 0.509198 0.476322 0.313143 0.023 Uiso calc 1 . . N N2 1.00317(13) 0.31909(9) 0.44361(9) 0.0218(3) Uani d 1 . . C C1 0.36530(18) 0.41720(11) 0.03233(11) 0.0271(4) Uani d 1 . . H H1A 0.386452 0.471272 0.007264 0.033 Uiso calc 1 . . H H1B 0.295614 0.388345 -0.011684 0.033 Uiso calc 1 . . C C2 0.48411(18) 0.36222(11) 0.05648(12) 0.0293(4) Uani d 1 . . H H2A 0.467461 0.313087 0.091029 0.035 Uiso calc 1 . . H H2B 0.506046 0.340649 0.003262 0.035 Uiso calc 1 . . C C3 0.71222(18) 0.36847(12) 0.12258(13) 0.0328(4) Uani d 1 . . H H3A 0.731332 0.351745 0.066887 0.039 Uiso calc 1 . . H H3B 0.709781 0.316629 0.157320 0.039 Uiso calc 1 . . C C4 0.81533(18) 0.42756(13) 0.17143(13) 0.0341(4) Uani d 1 . . H H4A 0.902653 0.401462 0.179119 0.041 Uiso calc 1 . . H H4B 0.813402 0.481006 0.138420 0.041 Uiso calc 1 . . C C5 0.88434(16) 0.50245(12) 0.30531(13) 0.0331(4) Uani d 1 . . H H5A 0.876221 0.558584 0.276532 0.040 Uiso calc 1 . . H H5B 0.974082 0.481140 0.310625 0.040 Uiso calc 1 . . C C6 0.85948(16) 0.51058(12) 0.39312(13) 0.0318(4) Uani d 1 . . H H6A 0.863463 0.454107 0.420879 0.038 Uiso calc 1 . . H H6B 0.926849 0.547190 0.430437 0.038 Uiso calc 1 . . C C7 0.69666(18) 0.54961(12) 0.46455(11) 0.0305(4) Uani d 1 . . H H7A 0.768173 0.574885 0.510153 0.037 Uiso calc 1 . . H H7B 0.680525 0.491440 0.482836 0.037 Uiso calc 1 . . C C8 0.57550(19) 0.60187(12) 0.45291(12) 0.0317(4) Uani d 1 . . H H8A 0.555432 0.611015 0.509943 0.038 Uiso calc 1 . . H H8B 0.588645 0.657881 0.428267 0.038 Uiso calc 1 . . C C9 0.35467(17) 0.61023(11) 0.37138(12) 0.0273(4) Uani d 1 . . H H9A 0.371993 0.660247 0.338265 0.033 Uiso calc 1 . . H H9B 0.330740 0.630519 0.424397 0.033 Uiso calc 1 . . C C10 0.24474(17) 0.55937(11) 0.31668(11) 0.0269(4) Uani d 1 . . H H10A 0.236833 0.504678 0.345546 0.032 Uiso calc 1 . . H H10B 0.161409 0.590616 0.309041 0.032 Uiso calc 1 . . C C11 0.16911(16) 0.49877(11) 0.17603(12) 0.0266(4) Uani d 1 . . H H11A 0.086447 0.531239 0.165171 0.032 Uiso calc 1 . . H H11B 0.155649 0.443498 0.202035 0.032 Uiso calc 1 . . C C12 0.20748(16) 0.48523(11) 0.09237(11) 0.0271(4) Uani d 1 . . H H12A 0.135557 0.457089 0.049429 0.033 Uiso calc 1 . . H H12B 0.225535 0.540395 0.067996 0.033 Uiso calc 1 . . C C13 0.52137(15) 0.35315(10) 0.29647(10) 0.0182(3) Uani d 1 . . C C14 0.63587(16) 0.31321(11) 0.33975(11) 0.0228(3) Uani d 1 . . H H14 0.715431 0.344133 0.355477 0.027 Uiso calc 1 . . C C15 0.63369(16) 0.22753(11) 0.36006(12) 0.0256(4) Uani d 1 . . H H15 0.711454 0.199452 0.390045 0.031 Uiso calc 1 . . C C16 0.51775(17) 0.18411(10) 0.33622(11) 0.0223(3) Uani d 1 . . C C17 0.40358(15) 0.22492(10) 0.29512(10) 0.0204(3) Uani d 1 . . C C18 0.40318(16) 0.30971(10) 0.27460(10) 0.0210(3) Uani d 1 . . H H18 0.324460 0.337741 0.246310 0.025 Uiso calc 1 . . C C19 0.9799(2) 0.21808(13) 0.30440(13) 0.0386(5) Uani d 1 . . H H19A 0.903305 0.250644 0.273509 0.058 Uiso calc 1 . . H H19B 0.951656 0.170727 0.335318 0.058 Uiso calc 1 . . H H19C 1.025720 0.196027 0.262443 0.058 Uiso calc 1 . . C C20 1.12006(16) 0.24739(11) 0.59910(11) 0.0241(4) Uani d 1 . . H H20A 1.102755 0.215876 0.648274 0.036 Uiso calc 1 . . H H20B 1.156054 0.303224 0.619071 0.036 Uiso calc 1 . . H H20C 1.183023 0.216001 0.575068 0.036 Uiso calc 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 S1 0.0245(2) 0.0200(2) 0.0237(2) 0.00381(16) 0.00752(16) 0.00348(16) S2 0.0185(2) 0.0215(2) 0.0230(2) 0.00144(15) 0.00544(15) -0.00034(16) F1 0.0340(6) 0.0179(5) 0.0359(6) 0.0003(4) 0.0115(4) 0.0055(4) F2 0.0245(5) 0.0250(5) 0.0313(5) -0.0080(4) 0.0027(4) 0.0001(4) O1 0.0245(6) 0.0224(6) 0.0207(6) -0.0003(5) 0.0037(5) 0.0026(5) O2 0.0289(6) 0.0221(6) 0.0296(6) 0.0022(5) 0.0104(5) -0.0007(5) O3 0.0208(6) 0.0274(7) 0.0357(7) -0.0018(5) 0.0103(5) 0.0038(5) O4 0.0208(6) 0.0262(6) 0.0274(6) 0.0015(5) -0.0001(5) 0.0034(5) O5 0.0259(6) 0.0219(6) 0.0263(6) -0.0011(5) 0.0066(5) -0.0035(5) O6 0.0216(6) 0.0289(7) 0.0285(6) -0.0034(5) 0.0089(5) -0.0013(5) O7 0.0326(7) 0.0258(7) 0.0303(7) -0.0034(5) 0.0097(5) 0.0058(5) O8 0.0388(8) 0.0511(9) 0.0355(7) 0.0251(7) 0.0176(6) 0.0161(7) O9 0.0289(6) 0.0240(6) 0.0289(6) -0.0068(5) 0.0073(5) -0.0006(5) O10 0.0274(7) 0.0393(8) 0.0337(7) 0.0098(6) 0.0126(5) -0.0014(6) N1 0.0192(7) 0.0171(7) 0.0206(7) 0.0002(5) 0.0038(5) -0.0006(5) N2 0.0239(7) 0.0173(7) 0.0239(7) 0.0037(5) 0.0054(6) 0.0009(6) C1 0.0353(10) 0.0260(9) 0.0194(8) -0.0097(8) 0.0054(7) -0.0005(7) C2 0.0434(11) 0.0218(9) 0.0265(9) -0.0057(8) 0.0159(8) -0.0058(7) C3 0.0371(10) 0.0311(10) 0.0354(10) 0.0122(8) 0.0191(8) 0.0034(8) C4 0.0283(10) 0.0375(11) 0.0418(11) 0.0079(8) 0.0191(8) 0.0120(9) C5 0.0161(8) 0.0218(9) 0.0606(13) -0.0011(7) 0.0085(8) 0.0039(9) C6 0.0195(8) 0.0218(9) 0.0461(11) 0.0020(7) -0.0067(8) 0.0001(8) C7 0.0338(10) 0.0291(10) 0.0239(9) -0.0079(8) -0.0016(7) 0.0012(7) C8 0.0402(10) 0.0289(10) 0.0267(9) -0.0097(8) 0.0096(8) -0.0093(8) C9 0.0336(10) 0.0210(9) 0.0317(9) 0.0057(7) 0.0164(8) 0.0014(7) C10 0.0253(9) 0.0277(9) 0.0311(9) 0.0056(7) 0.0136(7) 0.0056(7) C11 0.0169(8) 0.0222(9) 0.0387(10) 0.0002(7) 0.0035(7) 0.0029(7) C12 0.0235(8) 0.0228(9) 0.0297(9) -0.0012(7) -0.0034(7) 0.0045(7) C13 0.0212(8) 0.0165(8) 0.0175(8) -0.0001(6) 0.0063(6) 0.0000(6) C14 0.0193(8) 0.0235(9) 0.0248(8) -0.0013(7) 0.0040(6) 0.0022(7) C15 0.0216(8) 0.0247(9) 0.0300(9) 0.0042(7) 0.0056(7) 0.0074(7) C16 0.0296(9) 0.0163(8) 0.0229(8) 0.0006(7) 0.0102(7) 0.0030(6) C17 0.0199(8) 0.0217(8) 0.0197(8) -0.0047(6) 0.0052(6) -0.0027(6) C18 0.0191(8) 0.0213(8) 0.0218(8) 0.0018(6) 0.0036(6) 0.0016(7) C19 0.0565(13) 0.0329(11) 0.0301(10) -0.0170(10) 0.0176(9) -0.0088(8) C20 0.0246(9) 0.0249(9) 0.0217(8) 0.0015(7) 0.0036(7) 0.0015(7) 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 -1 0 0 -1 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 4 0 0 4 0 0 -4 0 0 -4 0 0 -5 0 0 5 0 0 5 0 0 -5 0 0 6 0 0 6 0 0 -7 0 0 7 0 0 -8 0 0 8 0 0 8 0 0 9 0 0 -9 0 0 10 0 0 -10 0 0 -11 0 0 -11 0 0 -12 0 0 -12 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 -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 1 0 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 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 -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 -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 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 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 -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 -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 16 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 2 0 0 2 0 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 -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 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 -5 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 9 0 -2 -9 0 2 -9 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 -12 0 -2 -12 0 -2 12 0 2 -12 0 -2 -12 0 2 -13 0 -2 -13 0 -2 -13 0 2 -13 0 -2 13 0 -2 -14 0 2 -14 0 2 14 0 -2 14 0 2 14 0 2 -14 0 -2 -14 0 2 -15 0 -2 -15 0 -2 15 0 2 15 0 -2 -16 0 2 -16 0 -2 16 0 2 16 0 -2 -16 0 -2 16 0 2 -17 0 -2 -17 0 -2 -17 0 -2 17 0 -2 17 0 -2 -18 0 -2 18 0 3 0 0 3 0 0 3 0 0 -3 0 0 3 0 0 3 1 0 -3 -1 0 3 -1 0 -3 1 0 3 1 0 3 -1 0 -3 1 0 3 1 0 3 1 0 3 -1 0 -3 -2 0 3 -2 0 3 2 0 3 -2 0 3 2 0 3 -2 0 -3 2 0 3 2 0 3 2 0 3 -3 0 3 -3 0 -3 3 0 3 3 0 3 3 0 -3 -3 0 3 -3 0 3 -3 0 3 3 0 3 3 0 3 3 0 -3 3 0 -3 3 0 -3 -4 0 3 -4 0 -3 4 0 3 4 0 3 -4 0 3 -4 0 3 -4 0 3 4 0 3 4 0 3 4 0 3 4 0 -3 4 0 3 5 0 3 5 0 3 5 0 3 5 0 3 5 0 3 -5 0 3 -5 0 3 -5 0 -3 5 0 3 5 0 3 -6 0 3 -6 0 3 6 0 3 6 0 3 -6 0 -3 -6 0 3 6 0 3 6 0 3 -6 0 3 -7 0 3 -7 0 3 7 0 3 -7 0 3 -7 0 3 7 0 -3 -7 0 3 8 0 -3 -8 0 3 -8 0 3 8 0 3 -8 0 3 -8 0 3 9 0 3 9 0 -3 9 0 3 -9 0 -3 -9 0 3 -9 0 3 -10 0 3 10 0 3 -10 0 -3 -10 0 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0 5 -14 0 -5 -14 0 -5 15 0 -5 -15 0 -5 -15 0 5 -15 0 -5 16 0 -5 16 0 -5 -16 0 -5 -16 0 5 -16 0 -5 17 0 -5 -17 0 5 -17 0 -5 17 0 -5 -17 0 -5 -18 0 -5 18 0 6 0 0 6 0 0 6 0 0 -6 1 0 6 -1 0 6 1 0 6 1 0 6 1 0 6 -1 0 6 1 0 6 2 0 6 -2 0 6 2 0 6 -2 0 6 2 0 6 -2 0 6 2 0 6 -2 0 6 2 0 -6 2 0 6 -3 0 6 -3 0 6 -3 0 6 3 0 6 3 0 6 3 0 6 3 0 6 3 0 6 -3 0 6 -4 0 6 4 0 6 -4 0 -6 4 0 -6 -4 0 6 4 0 6 4 0 6 4 0 6 -4 0 6 -5 0 6 -5 0 6 -5 0 6 5 0 -6 -5 0 -6 5 0 6 5 0 6 5 0 6 5 0 6 5 0 -6 6 0 -6 -6 0 -6 6 0 6 -6 0 6 6 0 6 6 0 6 6 0 6 -6 0 6 -6 0 6 7 0 6 7 0 6 -7 0 -6 7 0 -6 -7 0 6 -7 0 6 7 0 6 -7 0 6 7 0 6 -8 0 6 -8 0 6 8 0 6 8 0 -6 8 0 -6 -8 0 6 8 0 6 -9 0 6 9 0 6 9 0 -6 -9 0 6 9 0 -6 9 0 6 -9 0 6 10 0 6 10 0 -6 -10 0 6 -10 0 -6 10 0 6 10 0 6 11 0 6 11 0 -6 11 0 -6 -11 0 6 -11 0 -6 12 0 6 12 0 6 12 0 6 13 0 -6 -13 0 6 -13 0 -6 13 0 -6 -13 0 -6 14 0 6 -14 0 -6 -14 0 -6 15 0 -6 -15 0 -6 -15 0 6 -15 0 -6 -16 0 6 -16 0 -6 -16 0 -6 16 0 -6 16 0 -6 17 0 -6 -17 0 -6 -18 0 7 0 0 7 0 0 7 0 0 7 1 0 7 -1 0 7 -1 0 7 1 0 7 1 0 7 1 0 7 1 0 7 2 0 7 -2 0 7 -2 0 7 2 0 7 -2 0 7 2 0 7 2 0 7 -2 0 7 3 0 -7 3 0 7 3 0 7 -3 0 7 -3 0 7 3 0 7 3 0 7 -3 0 7 -4 0 7 -4 0 -7 4 0 7 -4 0 7 4 0 7 4 0 7 -4 0 7 4 0 7 4 0 7 4 0 7 -5 0 7 -5 0 7 5 0 7 5 0 -7 5 0 7 5 0 -7 -5 0 -7 5 0 7 -5 0 7 6 0 7 6 0 -7 6 0 7 6 0 -7 -6 0 7 -6 0 7 -6 0 7 -7 0 7 7 0 7 -7 0 7 -7 0 7 7 0 -7 -7 0 7 7 0 7 7 0 -7 7 0 7 -8 0 7 8 0 7 -8 0 7 -8 0 7 8 0 -7 8 0 7 8 0 -7 -8 0 -7 -9 0 7 9 0 7 -9 0 7 9 0 7 9 0 -7 9 0 7 -9 0 7 10 0 -7 -10 0 7 10 0 7 -10 0 7 10 0 -7 10 0 -7 -11 0 7 -11 0 7 11 0 7 11 0 -7 11 0 7 12 0 -7 -12 0 7 -12 0 7 13 0 7 -13 0 -7 -13 0 -7 13 0 -7 -13 0 7 -14 0 -7 14 0 -7 14 0 -7 -14 0 -7 -15 0 7 -15 0 -7 15 0 -7 15 0 -7 -16 0 -7 16 0 7 -16 0 -7 16 0 -7 -17 0 -7 17 0 8 0 0 8 0 0 8 0 0 8 0 0 8 -1 0 8 1 0 8 1 0 8 -1 0 8 1 0 8 -1 0 8 2 0 8 2 0 8 2 0 8 2 0 8 2 0 8 -2 0 8 -2 0 8 2 0 8 -2 0 8 3 0 8 -3 0 -8 3 0 8 3 0 8 3 0 8 -3 0 8 3 0 8 3 0 8 -3 0 8 4 0 -8 4 0 8 4 0 8 4 0 8 -4 0 8 -4 0 8 4 0 8 -5 0 8 5 0 -8 5 0 8 5 0 8 5 0 8 -5 0 8 -5 0 8 -6 0 8 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-11 -1 10 -11 1 10 -11 -1 10 -11 1 10 -11 -1 10 -11 1 9 -11 -1 9 -11 1 9 -11 -1 9 -11 1 9 -11 -1 9 -11 1 9 -11 -1 9 -11 1 8 -11 -1 8 -11 1 8 -11 -1 8 -11 1 8 -11 -1 8 -11 1 8 -11 -1 8 -11 1 7 -11 -1 7 -11 1 7 -11 -1 7 -11 1 7 -11 1 7 -11 -1 7 -11 -1 6 -11 1 6 -11 -1 6 -11 1 6 -11 -1 6 -11 1 5 -11 -1 5 -11 -1 5 -11 1 5 -11 -1 5 -11 1 4 -11 -1 4 -11 1 4 -11 1 4 -11 -1 4 -11 1 4 -11 -1 4 -11 1 3 -11 1 3 -11 -1 3 -11 1 3 -11 -1 3 -11 1 3 -11 1 3 -11 -1 3 -11 -1 3 -11 1 2 -11 -1 2 -11 -1 2 -11 1 2 -11 1 2 -11 -1 2 -11 -1 2 -11 1 2 -11 -1 1 -11 1 1 -11 -1 1 -11 -1 1 -11 1 1 -11 1 1 -11 -1 1 -11 1 1 -11 -1 1 -11 -1 0 -11 1 0 -11 1 0 -11 -1 0 -11 -1 0 -11 1 0 -11 1 0 -11 -1 0 -11 -1 0 -11 1 0 -11 -1 -1 -11 1 -1 -11 1 -1 -11 -1 -1 -11 -1 -1 -11 -1 -1 -11 -1 -1 -11 1 -1 -11 -1 -2 -11 1 -2 -11 1 -2 -11 -1 -2 -11 -1 -2 -11 1 -2 -11 -1 -3 -11 1 -3 -11 1 -3 -11 -1 -3 -11 -1 -3 -11 1 -3 -11 1 -4 -11 -1 -4 -11 1 -4 -11 -1 -4 -11 -1 -5 -11 1 -5 -11 1 -5 -11 -1 -5 -11 -2 14 -11 2 14 -11 -2 13 -11 2 13 -11 -2 13 -11 2 12 -11 2 12 -11 -2 12 -11 2 12 -11 -2 12 -11 2 11 -11 -2 11 -11 2 11 -11 -2 11 -11 2 11 -11 -2 11 -11 2 10 -11 -2 10 -11 2 10 -11 -2 10 -11 -2 10 -11 -2 10 -11 2 10 -11 2 9 -11 -2 9 -11 -2 9 -11 2 9 -11 -2 9 -11 2 9 -11 -2 9 -11 2 8 -11 -2 8 -11 2 8 -11 -2 8 -11 2 8 -11 2 8 -11 -2 8 -11 -2 8 -11 2 7 -11 2 7 -11 -2 7 -11 2 7 -11 -2 7 -11 2 7 -11 -2 7 -11 2 6 -11 2 6 -11 -2 6 -11 -2 6 -11 2 6 -11 -2 6 -11 2 5 -11 -2 5 -11 2 5 -11 2 5 -11 -2 5 -11 -2 5 -11 2 4 -11 -2 4 -11 2 4 -11 2 4 -11 -2 4 -11 -2 4 -11 -2 3 -11 2 3 -11 2 3 -11 -2 3 -11 2 3 -11 -2 3 -11 -2 3 -11 2 3 -11 -2 3 -11 2 2 -11 -2 2 -11 2 2 -11 -2 2 -11 -2 2 -11 -2 2 -11 2 2 -11 2 1 -11 -2 1 -11 2 1 -11 -2 1 -11 -2 1 -11 -2 1 -11 2 1 -11 2 0 -11 -2 0 -11 -2 0 -11 -2 0 -11 -2 0 -11 2 0 -11 2 -1 -11 -2 -1 -11 -2 -1 -11 -2 -1 -11 -2 -1 -11 2 -1 -11 -2 -2 -11 -2 -2 -11 2 -2 -11 -2 -2 -11 2 -2 -11 -2 -3 -11 2 -3 -11 -2 -3 -11 2 -3 -11 -2 -3 -11 2 -4 -11 -2 -4 -11 -2 -4 -11 -2 -5 -11 2 -5 -11 2 -5 -11 -3 13 -11 3 13 -11 -3 13 -11 -3 12 -11 -3 12 -11 3 12 -11 3 12 -11 3 11 -11 -3 11 -11 -3 11 -11 3 11 -11 -3 11 -11 3 11 -11 3 10 -11 -3 10 -11 -3 10 -11 3 10 -11 -3 10 -11 3 10 -11 -3 10 -11 3 9 -11 -3 9 -11 3 9 -11 -3 9 -11 3 9 -11 -3 9 -11 -3 9 -11 3 8 -11 -3 8 -11 3 8 -11 -3 8 -11 -3 8 -11 3 7 -11 3 7 -11 -3 7 -11 3 7 -11 -3 7 -11 -3 7 -11 3 6 -11 3 6 -11 -3 6 -11 -3 6 -11 3 6 -11 -3 6 -11 -3 5 -11 3 5 -11 -3 5 -11 3 5 -11 -3 5 -11 3 4 -11 3 4 -11 -3 4 -11 -3 4 -11 3 4 -11 -3 4 -11 3 3 -11 3 3 -11 -3 3 -11 3 3 -11 -3 3 -11 -3 3 -11 -3 3 -11 3 2 -11 -3 2 -11 3 2 -11 -3 2 -11 -3 2 -11 -3 2 -11 3 2 -11 3 1 -11 -3 1 -11 3 1 -11 -3 1 -11 -3 1 -11 -3 1 -11 3 1 -11 3 0 -11 -3 0 -11 -3 0 -11 -3 0 -11 -3 0 -11 3 0 -11 3 -1 -11 -3 -1 -11 -3 -1 -11 3 -1 -11 -3 -1 -11 -3 -1 -11 3 -2 -11 -3 -2 -11 -3 -2 -11 3 -2 -11 3 -3 -11 -3 -3 -11 -3 -3 -11 3 -3 -11 3 -4 -11 -3 -4 -11 3 -4 -11 3 -5 -11 -3 -5 -11 4 13 -11 -4 13 -11 4 12 -11 -4 12 -11 -4 12 -11 4 11 -11 -4 11 -11 -4 11 -11 4 10 -11 -4 10 -11 4 10 -11 -4 10 -11 -4 10 -11 -4 10 -11 4 9 -11 4 9 -11 -4 9 -11 -4 9 -11 4 8 -11 -4 8 -11 4 8 -11 -4 8 -11 -4 8 -11 -4 7 -11 4 7 -11 -4 7 -11 4 7 -11 -4 7 -11 -4 6 -11 4 6 -11 4 6 -11 -4 6 -11 -4 6 -11 4 6 -11 4 5 -11 -4 5 -11 4 5 -11 -4 5 -11 -4 5 -11 -4 4 -11 4 4 -11 -4 4 -11 4 4 -11 -4 4 -11 -4 3 -11 4 3 -11 -4 3 -11 -4 3 -11 4 3 -11 -4 3 -11 4 2 -11 4 2 -11 -4 2 -11 4 2 -11 -4 2 -11 -4 2 -11 -4 1 -11 4 1 -11 4 1 -11 -4 1 -11 -4 1 -11 -4 1 -11 -4 0 -11 4 0 -11 4 0 -11 -4 0 -11 -4 0 -11 -4 0 -11 -4 -1 -11 -4 -1 -11 4 -1 -11 -4 -1 -11 -4 -1 -11 4 -1 -11 -4 -2 -11 4 -2 -11 4 -2 -11 -4 -2 -11 4 -3 -11 -4 -3 -11 -4 -3 -11 4 -3 -11 4 -4 -11 -4 -4 -11 4 -5 -11 -4 -5 -11 5 13 -11 5 12 -11 -5 12 -11 -5 12 -11 5 11 -11 -5 11 -11 5 10 -11 -5 10 -11 5 9 -11 -5 9 -11 -5 9 -11 -5 8 -11 -5 8 -11 5 8 -11 5 8 -11 -5 8 -11 -5 7 -11 -5 7 -11 5 7 -11 5 7 -11 -5 7 -11 -5 6 -11 -5 6 -11 5 6 -11 5 6 -11 -5 6 -11 -5 5 -11 -5 5 -11 -5 5 -11 -5 4 -11 -5 4 -11 -5 4 -11 -5 3 -11 -5 3 -11 -5 3 -11 -5 3 -11 5 2 -11 -5 2 -11 -5 2 -11 -5 2 -11 -5 1 -11 5 1 -11 -5 1 -11 -5 1 -11 -5 1 -11 -5 0 -11 -5 0 -11 5 0 -11 -5 0 -11 -5 0 -11 -5 -1 -11 5 -1 -11 -5 -1 -11 -5 -1 -11 -5 -1 -11 -5 -2 -11 5 -2 -11 -5 -2 -11 -5 -2 -11 5 -3 -11 -5 -3 -11 5 -4 -11 -5 -4 -11 6 12 -11 6 11 -11 -6 11 -11 6 10 -11 -6 10 -11 6 9 -11 -6 9 -11 -6 9 -11 -6 8 -11 -6 8 -11 6 8 -11 -6 8 -11 -6 7 -11 -6 7 -11 6 7 -11 -6 7 -11 -6 6 -11 -6 6 -11 -6 6 -11 -6 5 -11 -6 5 -11 -6 5 -11 -6 4 -11 -6 4 -11 -6 3 -11 -6 3 -11 -6 2 -11 -6 2 -11 -6 2 -11 6 1 -11 -6 1 -11 -6 1 -11 -6 1 -11 6 0 -11 -6 0 -11 -6 0 -11 -6 0 -11 -6 -1 -11 6 -1 -11 -6 -1 -11 -6 -1 -11 -6 -2 -11 -6 -2 -11 -6 -3 -11 6 -3 -11 -6 -4 -11 6 -4 -11 -7 11 -11 -7 10 -11 -7 9 -11 -7 8 -11 -7 8 -11 -7 7 -11 -7 7 -11 -7 7 -11 -7 6 -11 -7 6 -11 -7 6 -11 -7 5 -11 -7 5 -11 -7 5 11 7 -4 -11 -7 4 -11 -7 4 -11 -7 4 -11 -7 3 -11 -7 3 -11 -7 2 -11 -7 2 -11 -7 1 -11 -7 1 -11 -7 0 -11 -7 0 -11 -7 -1 -11 7 -1 -11 -7 -2 -11 -7 -2 -11 7 -2 -11 -7 -3 -11 -8 10 -11 -8 9 -11 -8 8 -11 -8 7 -11 -8 7 -11 -8 6 -11 -8 6 -11 -8 5 -11 -8 5 -11 -8 5 -11 -8 4 -11 -8 4 11 8 -4 -11 -8 4 -11 -8 3 -11 -8 3 11 8 -3 -11 -8 2 -11 -8 2 11 8 -2 -11 -8 1 -11 -8 0 -11 -8 -1 -11 -9 9 11 9 -9 -11 -9 8 -11 -9 7 -11 -9 6 -11 -9 6 11 9 -5 -11 -9 5 -11 -9 5 11 9 -4 -11 -9 4 11 9 -3 -11 -9 3 11 9 -2 -11 -9 2 -11 -9 1 -11 -9 0 -11 -10 6 -11 -10 5 -11 -10 3 -11 -10 2 -12 0 11 -12 0 10 -12 0 9 -12 0 8 -12 0 8 -12 0 7 -12 0 7 -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 1 -12 0 0 -12 0 0 -12 0 -1 -12 0 -1 -12 0 -2 -12 1 11 -12 1 11 -12 -1 11 -12 1 10 -12 -1 10 -12 -1 9 -12 1 9 -12 -1 9 -12 -1 8 -12 1 8 -12 -1 8 -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 5 -12 -1 5 -12 -1 5 -12 1 4 -12 -1 4 -12 1 3 -12 -1 3 -12 -1 3 -12 -1 2 -12 1 2 -12 -1 2 -12 1 2 -12 -1 1 -12 -1 1 -12 1 1 -12 -1 0 -12 1 0 -12 1 0 -12 -1 -1 -12 1 -1 -12 1 -1 -12 -1 -2 -12 1 -2 -12 2 11 -12 2 11 -12 2 10 -12 -2 10 -12 -2 9 -12 2 9 -12 -2 9 -12 -2 8 -12 2 8 -12 -2 8 -12 -2 7 -12 -2 7 -12 2 7 -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 4 -12 -2 4 -12 -2 4 -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 0 -12 -2 0 -12 2 0 -12 -2 -1 -12 2 -1 -12 2 -2 -12 -2 -2 -12 2 -2 -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 7 -12 3 7 -12 -3 7 -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 2 -12 -3 2 -12 -3 1 -12 3 0 -12 -3 0 -12 -3 -1 -12 3 -1 -12 3 -2 -12 -3 -2 -12 -4 10 -12 4 10 -12 -4 9 -12 -4 9 -12 -4 8 -12 -4 8 -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 4 -12 -4 3 -12 -4 3 -12 -4 2 -12 -4 1 -12 -4 0 -12 -4 -1 -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 4 -12 -5 3 -12 -5 2 -12 -5 1 -12 -5 0 -12 -6 9 -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 -7 5 -12 -7 4 -12 -7 3 -12 -7 2 -13 -1 6 -13 -1 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 O7 S1 N2 . . 107.44(7) ? O7 S1 C19 . . 106.06(9) ? O8 S1 O7 . . 115.20(8) ? O8 S1 N2 . . 112.67(8) ? O8 S1 C19 . . 108.48(10) ? N2 S1 C19 . . 106.44(9) ? O9 S2 N2 . . 113.27(7) ? O9 S2 C20 . . 106.38(8) ? O10 S2 O9 . . 115.82(8) ? O10 S2 N2 . . 106.41(8) ? O10 S2 C20 . . 106.77(8) ? N2 S2 C20 . . 107.78(8) ? C12 O1 C1 . . 111.97(12) ? C2 O2 C3 . . 113.10(14) ? C4 O3 C5 . . 112.73(13) ? C7 O4 C6 . . 111.85(13) ? C9 O5 C8 . . 111.75(13) ? C11 O6 C10 . . 112.50(12) ? H1C N1 H1D . . 109.5 ? H1C N1 H1E . . 109.5 ? H1D N1 H1E . . 109.5 ? C13 N1 H1C . . 109.5 ? C13 N1 H1D . . 109.5 ? C13 N1 H1E . . 109.5 ? S1 N2 S2 . . 120.73(9) ? O1 C1 H1A . . 110.1 ? O1 C1 H1B . . 110.1 ? O1 C1 C2 . . 108.17(13) ? H1A C1 H1B . . 108.4 ? C2 C1 H1A . . 110.1 ? C2 C1 H1B . . 110.1 ? O2 C2 C1 . . 108.55(14) ? O2 C2 H2A . . 110.0 ? O2 C2 H2B . . 110.0 ? C1 C2 H2A . . 110.0 ? C1 C2 H2B . . 110.0 ? H2A C2 H2B . . 108.4 ? O2 C3 H3A . . 110.1 ? O2 C3 H3B . . 110.1 ? O2 C3 C4 . . 108.01(15) ? H3A C3 H3B . . 108.4 ? C4 C3 H3A . . 110.1 ? C4 C3 H3B . . 110.1 ? O3 C4 C3 . . 108.75(14) ? O3 C4 H4A . . 109.9 ? O3 C4 H4B . . 109.9 ? C3 C4 H4A . . 109.9 ? C3 C4 H4B . . 109.9 ? H4A C4 H4B . . 108.3 ? O3 C5 H5A . . 109.9 ? O3 C5 H5B . . 109.9 ? O3 C5 C6 . . 109.11(14) ? H5A C5 H5B . . 108.3 ? C6 C5 H5A . . 109.9 ? C6 C5 H5B . . 109.9 ? O4 C6 C5 . . 108.64(14) ? O4 C6 H6A . . 110.0 ? O4 C6 H6B . . 110.0 ? C5 C6 H6A . . 110.0 ? C5 C6 H6B . . 110.0 ? H6A C6 H6B . . 108.3 ? O4 C7 H7A . . 110.0 ? O4 C7 H7B . . 110.0 ? O4 C7 C8 . . 108.45(14) ? H7A C7 H7B . . 108.4 ? C8 C7 H7A . . 110.0 ? C8 C7 H7B . . 110.0 ? O5 C8 C7 . . 108.95(14) ? O5 C8 H8A . . 109.9 ? O5 C8 H8B . . 109.9 ? C7 C8 H8A . . 109.9 ? C7 C8 H8B . . 109.9 ? H8A C8 H8B . . 108.3 ? O5 C9 H9A . . 109.8 ? O5 C9 H9B . . 109.8 ? O5 C9 C10 . . 109.23(14) ? H9A C9 H9B . . 108.3 ? C10 C9 H9A . . 109.8 ? C10 C9 H9B . . 109.8 ? O6 C10 C9 . . 108.49(13) ? O6 C10 H10A . . 110.0 ? O6 C10 H10B . . 110.0 ? C9 C10 H10A . . 110.0 ? C9 C10 H10B . . 110.0 ? H10A C10 H10B . . 108.4 ? O6 C11 H11A . . 110.0 ? O6 C11 H11B . . 110.0 ? O6 C11 C12 . . 108.27(13) ? H11A C11 H11B . . 108.4 ? C12 C11 H11A . . 110.0 ? C12 C11 H11B . . 110.0 ? O1 C12 C11 . . 108.41(13) ? O1 C12 H12A . . 110.0 ? O1 C12 H12B . . 110.0 ? C11 C12 H12A . . 110.0 ? C11 C12 H12B . . 110.0 ? H12A C12 H12B . . 108.4 ? C14 C13 N1 . . 119.90(14) ? C14 C13 C18 . . 121.25(15) ? C18 C13 N1 . . 118.82(14) ? C13 C14 H14 . . 120.2 ? C13 C14 C15 . . 119.60(15) ? C15 C14 H14 . . 120.2 ? C14 C15 H15 . . 120.4 ? C16 C15 C14 . . 119.12(16) ? C16 C15 H15 . . 120.4 ? F1 C16 C15 . . 120.83(15) ? F1 C16 C17 . . 118.30(15) ? C15 C16 C17 . . 120.86(15) ? F2 C17 C16 . . 118.59(15) ? F2 C17 C18 . . 120.33(15) ? C18 C17 C16 . . 121.06(15) ? C13 C18 H18 . . 121.0 ? C17 C18 C13 . . 118.07(15) ? C17 C18 H18 . . 121.0 ? S1 C19 H19A . . 109.5 ? S1 C19 H19B . . 109.5 ? S1 C19 H19C . . 109.5 ? H19A C19 H19B . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? S2 C20 H20A . . 109.5 ? S2 C20 H20B . . 109.5 ? S2 C20 H20C . . 109.5 ? H20A C20 H20B . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? 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 S1 O7 . 1.4442(12) ? S1 O8 . 1.4436(13) ? S1 N2 . 1.5916(14) ? S1 C19 . 1.7571(19) ? S2 O9 . 1.4519(12) ? S2 O10 . 1.4429(12) ? S2 N2 . 1.5949(14) ? S2 C20 . 1.7620(17) ? F1 C16 . 1.3532(19) ? F2 C17 . 1.3435(18) ? O1 C1 . 1.436(2) ? O1 C12 . 1.428(2) ? O2 C2 . 1.425(2) ? O2 C3 . 1.426(2) ? O3 C4 . 1.425(2) ? O3 C5 . 1.433(2) ? O4 C6 . 1.435(2) ? O4 C7 . 1.422(2) ? O5 C8 . 1.434(2) ? O5 C9 . 1.432(2) ? O6 C10 . 1.428(2) ? O6 C11 . 1.428(2) ? N1 H1C . 0.9100 ? N1 H1D . 0.9100 ? N1 H1E . 0.9100 ? N1 C13 . 1.469(2) ? C1 H1A . 0.9900 ? C1 H1B . 0.9900 ? C1 C2 . 1.495(3) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C3 C4 . 1.495(3) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 H5A . 0.9900 ? C5 H5B . 0.9900 ? C5 C6 . 1.486(3) ? C6 H6A . 0.9900 ? C6 H6B . 0.9900 ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C7 C8 . 1.495(3) ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C9 C10 . 1.497(3) ? C10 H10A . 0.9900 ? C10 H10B . 0.9900 ? C11 H11A . 0.9900 ? C11 H11B . 0.9900 ? C11 C12 . 1.497(2) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C13 C14 . 1.385(2) ? C13 C18 . 1.391(2) ? C14 H14 . 0.9500 ? C14 C15 . 1.391(2) ? C15 H15 . 0.9500 ? C15 C16 . 1.372(2) ? C16 C17 . 1.379(2) ? C17 C18 . 1.376(2) ? C18 H18 . 0.9500 ? C19 H19A . 0.9800 ? C19 H19B . 0.9800 ? C19 H19C . 0.9800 ? C20 H20A . 0.9800 ? C20 H20B . 0.9800 ? C20 H20C . 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 N1 H1C O1 . 0.91 2.01 2.8925(17) 162.9 yes N1 H1D O3 . 0.91 2.02 2.8976(17) 162.3 yes N1 H1E O5 . 0.91 1.96 2.8614(17) 173.8 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 F1 C16 C17 F2 . . . . -1.0(2) ? F1 C16 C17 C18 . . . . -179.56(14) ? F2 C17 C18 C13 . . . . -178.51(14) ? O1 C1 C2 O2 . . . . -70.86(16) ? O2 C3 C4 O3 . . . . 64.63(18) ? O3 C5 C6 O4 . . . . -63.52(18) ? O4 C7 C8 O5 . . . . 67.19(18) ? O5 C9 C10 O6 . . . . -70.26(17) ? O6 C11 C12 O1 . . . . 63.66(17) ? O7 S1 N2 S2 . . . . -170.63(9) ? O8 S1 N2 S2 . . . . -42.68(13) ? O9 S2 N2 S1 . . . . -45.30(12) ? O10 S2 N2 S1 . . . . -173.68(9) ? N1 C13 C14 C15 . . . . -176.46(15) ? N1 C13 C18 C17 . . . . 176.29(14) ? C1 O1 C12 C11 . . . . 179.99(13) ? C2 O2 C3 C4 . . . . 177.42(14) ? C3 O2 C2 C1 . . . . -171.83(14) ? C4 O3 C5 C6 . . . . -174.88(14) ? C5 O3 C4 C3 . . . . -178.86(14) ? C6 O4 C7 C8 . . . . 170.06(14) ? C7 O4 C6 C5 . . . . 174.53(14) ? C8 O5 C9 C10 . . . . -175.86(13) ? C9 O5 C8 C7 . . . . -171.63(14) ? C10 O6 C11 C12 . . . . -178.88(13) ? C11 O6 C10 C9 . . . . -178.03(13) ? C12 O1 C1 C2 . . . . -179.59(13) ? C13 C14 C15 C16 . . . . 0.4(3) ? C14 C13 C18 C17 . . . . -1.7(2) ? C14 C15 C16 F1 . . . . 179.42(15) ? C14 C15 C16 C17 . . . . -2.1(3) ? C15 C16 C17 F2 . . . . -179.56(15) ? C15 C16 C17 C18 . . . . 1.9(2) ? C16 C17 C18 C13 . . . . 0.0(2) ? C18 C13 C14 C15 . . . . 1.5(2) ? C19 S1 N2 S2 . . . . 76.10(12) ? C20 S2 N2 S1 . . . . 72.11(11) ? _cod_database_fobs_code 2312736