#------------------------------------------------------------------------------ #$Date: 2024-06-18 04:55:57 +0300 (Tue, 18 Jun 2024) $ #$Revision: 292440 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/25/2312521.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_2312521 loop_ _publ_author_name 'Pickl, Thomas' 'Zuber, Julian' 'Stephan, Johannes' 'Pöthig, Alexander' _publ_section_title ; Crystal structure elucidation of a geminal and vicinal bis(trifluoromethanesulfonate) ester. ; _journal_coeditor_code OJ3019 _journal_issue 7 _journal_name_full 'Acta crystallographica. Section C, Structural chemistry' _journal_paper_doi 10.1107/S2053229624005230 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C4 H4 F6 O6 S2' _chemical_formula_sum 'C4 H4 F6 O6 S2' _chemical_formula_weight 326.19 _chemical_name_common ; Ethylene bis(triflate) ; _chemical_name_systematic ; Ethane-1,2-diyl bis(trifluoromethanesulfonate) ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method ; FinalCif V133 by Daniel Kratzert, Freiburg 2024, https://dkratzert.de/finalcif.html ; _cell_angle_alpha 83.540(9) _cell_angle_beta 64.178(9) _cell_angle_gamma 89.593(9) _cell_formula_units_Z 4 _cell_length_a 10.036(4) _cell_length_b 10.664(3) _cell_length_c 11.276(4) _cell_measurement_reflns_used 3670 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.344 _cell_measurement_theta_min 2.26 _cell_volume 1078.2(7) _computing_cell_refinement ; SAINT (Bruker, 2019) ; _computing_data_collection ; APEX4 (Bruker, 2022) ; _computing_data_reduction ; SAINT (Bruker, 2019) ; _computing_molecular_graphics ; PLATON (Spek, 2020) ; _computing_publication_material ; PLATON (Spek, 2020), enCIFer (Allen et al., 2004) and FinalCif (Kratzert, 2023) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) and SHELXLE (H\"ubschle et al., 2011) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_detector CPAD _diffrn_detector_area_resol_mean 16 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device 'three-angle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'Helios optic' _diffrn_radiation_probe x-ray _diffrn_radiation_source 'TXS rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_unetI/netI 0.0701 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4339 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_min 1.924 _diffrn_source 'TXS rotating anode' _diffrn_source_current 50.0 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_T_max 0.745373 _exptl_absorpt_correction_T_min 0.564122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (TWINABS; Bruker, 2012) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.009 _exptl_crystal_description plate _exptl_crystal_F_000 648 _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.012 _refine_diff_density_max 0.604 _refine_diff_density_min -0.548 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 326 _refine_ls_number_reflns 4339 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0658 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+5.6794P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1490 _refine_ls_wR_factor_ref 0.1657 _reflns_number_gt 3403 _reflns_number_total 4339 _reflns_threshold_expression 'I > 2\s(I)' _twin_individual_id 2 _twin_individual_twin_matrix_11 0.00071 _twin_individual_twin_matrix_12 -0.0027 _twin_individual_twin_matrix_13 -0.99868 _twin_individual_twin_matrix_21 0.95311 _twin_individual_twin_matrix_22 0.21903 _twin_individual_twin_matrix_23 -0.12083 _twin_individual_twin_matrix_31 0.41847 _twin_individual_twin_matrix_32 -0.95442 _twin_individual_twin_matrix_33 -0.02247 _iucr_refine_instructions_details ; TITL PicTh35_0m_4_b.res in P-1 PicTh35_0m_5.res created by SHELXL-2019/1 at 12:02:21 on 04-Sep-2023 CELL 0.71073 10.0356 10.6643 11.2760 83.540 64.178 89.593 ZERR 4.00 0.0035 0.0033 0.0040 0.009 0.009 0.009 LATT 1 SFAC C O F S H UNIT 16 24 24 8 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 L.S. 5 FMAP 2 ACTA PLAN 10 WGHT 0.0356 5.6795 BASF 0.37272 FVAR 0.51437 C1 1 0.738964 0.780569 -0.314510 11.00000 0.02644 0.03238 = 0.03350 -0.00424 -0.01371 -0.00045 C2 1 0.798102 0.542623 -0.095187 11.00000 0.03775 0.01760 = 0.05517 -0.01243 -0.02917 0.01095 AFIX 23 H2A 5 0.902806 0.520173 -0.141213 11.00000 -1.20000 H2B 5 0.739825 0.497232 -0.130181 11.00000 -1.20000 AFIX 0 C3 1 0.740760 0.503776 0.050529 11.00000 0.02828 0.01717 = 0.04602 -0.00538 -0.02573 0.00024 AFIX 23 H3A 5 0.642752 0.539256 0.098399 11.00000 -1.20000 H3B 5 0.728878 0.410543 0.069459 11.00000 -1.20000 AFIX 0 C4 1 0.703061 0.580681 0.348086 11.00000 0.04695 0.03241 = 0.03605 -0.00241 -0.02517 -0.00033 C5 1 0.858927 0.272599 0.625711 11.00000 0.03646 0.02363 = 0.03244 -0.00486 -0.01668 0.00569 C6 1 0.792749 0.099816 0.913818 11.00000 0.01936 0.01580 = 0.03402 -0.00097 -0.01475 0.00320 AFIX 23 H6A 5 0.899447 0.113447 0.889450 11.00000 -1.20000 H6B 5 0.782152 0.034746 0.862035 11.00000 -1.20000 AFIX 0 C7 1 0.711141 0.056400 1.057814 11.00000 0.02104 0.02380 = 0.03210 -0.00106 -0.01640 -0.00049 AFIX 23 H7A 5 0.753362 -0.021922 1.080005 11.00000 -1.20000 H7B 5 0.605728 0.037346 1.080766 11.00000 -1.20000 AFIX 0 C8 1 0.739035 0.066060 1.353370 11.00000 0.03915 0.03727 = 0.03519 -0.00476 -0.02019 -0.00152 O1 2 0.541628 0.637430 -0.111455 11.00000 0.02277 0.02093 = 0.05101 -0.00499 -0.01650 -0.00506 O2 2 0.615607 0.846998 -0.077976 11.00000 0.02673 0.01912 = 0.03507 -0.00482 -0.01035 0.00146 O3 2 0.786947 0.680016 -0.120796 11.00000 0.02624 0.02310 = 0.03782 -0.00242 -0.01930 0.00376 O4 2 0.847447 0.551171 0.096084 11.00000 0.02453 0.02159 = 0.04223 0.00033 -0.02200 0.00044 O5 2 0.714816 0.746732 0.154609 11.00000 0.03061 0.01918 = 0.04286 -0.00153 -0.02106 0.00544 O6 2 0.948096 0.701962 0.175925 11.00000 0.03238 0.03362 = 0.05649 0.00185 -0.02929 -0.01087 O7 2 0.626491 0.119242 0.753681 11.00000 0.03353 0.02235 = 0.04901 -0.00547 -0.02556 -0.00205 O8 2 0.602259 0.347753 0.786102 11.00000 0.02834 0.02142 = 0.04250 -0.00559 -0.01906 0.00856 O9 2 0.732330 0.218645 0.882920 11.00000 0.02174 0.01647 = 0.02846 -0.00339 -0.01136 0.00271 O10 2 0.722195 0.156100 1.135954 11.00000 0.02928 0.02468 = 0.03560 -0.00705 -0.02174 0.00924 O11 2 0.960769 0.079483 1.118966 11.00000 0.02430 0.03408 = 0.04368 -0.01108 -0.01890 0.00982 O12 2 0.861763 0.277606 1.211804 11.00000 0.03961 0.02570 = 0.04635 -0.00397 -0.02282 0.00453 F1 3 0.795633 0.681574 -0.379229 11.00000 0.05538 0.04812 = 0.03609 -0.01490 -0.01785 0.00755 F2 3 0.638310 0.827313 -0.353268 11.00000 0.05701 0.05893 = 0.04461 -0.00245 -0.03509 0.01271 F3 3 0.846727 0.868661 -0.348409 11.00000 0.04319 0.03734 = 0.03793 0.00694 -0.00774 -0.01087 F4 3 0.590843 0.512900 0.350265 11.00000 0.04664 0.05483 = 0.03748 0.00944 -0.01237 -0.02306 F5 3 0.784093 0.505067 0.385517 11.00000 0.06723 0.03557 = 0.05332 0.01243 -0.03447 -0.00153 F6 3 0.648565 0.664162 0.432046 11.00000 0.07154 0.04858 = 0.04166 -0.00744 -0.01968 0.00546 F7 3 0.838874 0.281918 0.515655 11.00000 0.05481 0.04012 = 0.02584 -0.00210 -0.01974 0.00101 F8 3 0.918982 0.380531 0.629962 11.00000 0.03360 0.03347 = 0.03597 -0.00106 -0.01198 -0.00975 F9 3 0.952081 0.181989 0.620240 11.00000 0.03030 0.03619 = 0.03239 -0.00034 -0.00558 0.01251 F10 3 0.686141 -0.044923 1.341981 11.00000 0.09099 0.04006 = 0.03973 0.01031 -0.02862 -0.03045 F11 3 0.626457 0.126950 1.430040 11.00000 0.03950 0.07195 = 0.03529 -0.00894 -0.00768 -0.00082 F12 3 0.827603 0.042770 1.411019 11.00000 0.07203 0.03818 = 0.04453 0.00634 -0.03792 -0.00105 S1 4 0.651292 0.733510 -0.137093 11.00000 0.01960 0.01745 = 0.02663 -0.00135 -0.01062 0.00050 S2 4 0.811475 0.661629 0.180554 11.00000 0.02575 0.01930 = 0.03299 0.00124 -0.01734 -0.00255 S3 4 0.681159 0.234931 0.770889 11.00000 0.02058 0.01884 = 0.03167 -0.00242 -0.01448 0.00192 S4 4 0.840457 0.153609 1.189724 11.00000 0.02513 0.01843 = 0.03010 -0.00130 -0.01473 0.00302 HKLF 5 1 1 0 0 0 1 0 0 0 1 REM PicTh35_0m_4_b.res in P-1 REM wR2 = 0.1657, GooF = S = 1.073, Restrained GooF = 1.073 for all data REM R1 = 0.0658 for 3403 Fo > 4sig(Fo) and 0.0941 for all 4339 data REM 326 parameters refined using 0 restraints END WGHT 0.0356 5.6795 REM Highest difference peak 0.604, deepest hole -0.548, 1-sigma level 0.128 Q1 1 0.6913 0.7403 -0.2330 11.00000 0.05 0.60 Q2 1 0.7594 0.2640 0.6598 11.00000 0.05 0.57 Q3 1 0.7770 0.1274 1.2848 11.00000 0.05 0.55 Q4 1 0.7472 0.6593 0.2908 11.00000 0.05 0.55 Q5 1 1.0329 0.0933 1.0007 11.00000 0.05 0.54 Q6 1 0.8780 0.6803 0.0650 11.00000 0.05 0.53 Q7 1 0.9406 0.5341 0.1116 11.00000 0.05 0.52 Q8 1 0.6586 0.1990 1.3829 11.00000 0.05 0.50 Q9 1 0.5859 0.7172 0.0008 11.00000 0.05 0.49 Q10 1 0.7013 0.3941 0.6897 11.00000 0.05 0.49 ; _cod_data_source_file oj3019.cif _cod_data_source_block 2 _cod_original_cell_volume 1078.2(6) _cod_database_code 2312521 _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_hkl_file ; 1 0 0 22.6464 0.98921 -2 1 0 0 22.6464 0.98921 1 3 0 0 23.9793 1.06507 1 4 0 0 499.135 9.63065 1 5 0 0 186.985 4.17691 1 6 1 0 266.208 11.2830 -2 6 0 0 266.208 11.2830 1 7 1 0 19.2053 3.84260 -2 7 0 0 19.2053 3.84260 1 8 1 0 230.646 8.91629 -2 8 0 0 230.646 8.91629 1 9 1 0 124.127 7.92268 -2 9 0 0 124.127 7.92268 1 10 1 0 30.2788 5.68611 -2 10 0 0 30.2788 5.68611 1 11 0 0 4.26151 6.73794 1 -11 1 0 -4.2246 4.71764 1 -10 1 0 25.2831 6.01033 1 9 2 1 78.2634 6.59100 -2 -9 1 0 78.2634 6.59100 1 8 2 1 75.0871 4.47095 -2 -8 1 0 75.0871 4.47095 1 7 2 1 56.8860 11.0086 -2 -7 1 0 56.8860 11.0086 1 -6 1 0 384.246 9.83935 1 -5 1 0 33.1892 1.71333 1 -4 1 0 182.933 4.13913 1 -3 1 0 89.6027 1.97365 1 -2 1 0 483.284 8.46130 1 -1 1 0 6.22084 0.40290 1 0 1 0 0.20398 0.30910 1 1 1 0 1.14471 0.37554 1 2 1 0 279.958 8.36022 1 3 1 0 837.356 15.9071 1 4 1 0 38.7649 1.77485 1 5 1 0 38.9955 2.06041 1 6 1 0 38.5247 3.88850 1 7 0 0 11.5520 4.16123 -2 7 1 0 11.5520 4.16123 1 8 0 0 281.207 10.2707 -2 8 1 0 281.207 10.2707 1 9 0 0 96.5981 8.00992 -2 9 1 0 96.5981 8.00992 1 10 0 0 41.4775 12.5515 -2 10 1 0 41.4775 12.5515 1 11 0 0 27.9406 15.2725 -2 11 1 0 27.9406 15.2725 1 11 3 1 53.7842 14.9787 -2 -11 2 0 53.7842 14.9787 1 10 3 1 44.9842 4.41102 -2 -10 2 0 44.9842 4.41102 1 9 3 1 14.1287 3.22415 -2 -9 2 0 14.1287 3.22415 1 8 3 1 3.50660 3.15397 -2 -8 2 0 3.50660 3.15397 1 7 3 1 141.956 5.83830 -2 -7 2 0 141.956 5.83830 1 6 3 1 482.303 31.8553 -2 -6 2 0 482.303 31.8553 1 -5 2 0 8.07583 0.85418 1 -4 2 0 391.462 7.39249 1 3 2 1 89.0916 8.57465 -2 -3 2 0 89.0916 8.57465 1 2 2 1 200.155 5.11145 -2 -2 2 0 200.155 5.11145 1 -1 2 0 2290.51 159.243 1 1 2 0 2809.72 191.929 1 -2 2 1 401.176 30.9914 -2 2 2 0 401.176 30.9914 1 3 2 0 691.302 15.1137 1 4 2 0 9.21881 1.30181 1 5 2 0 93.0960 2.86723 1 -6 1 1 17.8113 4.33623 -2 6 2 0 17.8113 4.33623 1 -7 1 1 308.389 16.2665 -2 7 2 0 308.389 16.2665 1 -8 1 1 139.887 12.8419 -2 8 2 0 139.887 12.8419 1 -9 1 1 4.89866 11.1054 -2 9 2 0 4.89866 11.1054 1 10 2 0 2.98589 2.42830 1 11 2 0 2.40463 2.43501 1 -11 3 0 1.03867 5.60575 1 10 4 1 56.7819 7.79365 -2 -10 3 0 56.7819 7.79365 1 9 4 1 17.8673 9.29572 -2 -9 3 0 17.8673 9.29572 1 -8 3 0 16.3825 2.56715 1 -7 3 0 2.95075 1.37724 1 -6 3 0 167.158 4.52473 1 -5 3 0 46.6967 1.83033 1 -4 3 0 15.6203 0.92462 1 -3 3 0 232.104 4.80422 1 -2 3 0 240.168 5.30915 1 -1 3 0 12.9957 0.75445 1 0 3 0 63.3972 1.89031 1 1 3 0 112.019 3.21360 1 2 3 0 38.1801 1.37114 1 3 3 0 50.2608 3.67933 1 4 3 0 184.833 4.77284 1 -5 2 1 68.1772 3.90884 -2 5 3 0 68.1772 3.90884 1 -6 2 1 338.650 9.76250 -2 6 3 0 338.650 9.76250 1 -7 2 1 293.081 9.66768 -2 7 3 0 293.081 9.66768 1 -8 2 1 153.445 6.47966 -2 8 3 0 153.445 6.47966 1 -9 2 1 72.7578 6.50404 -2 9 3 0 72.7578 6.50404 1 -10 2 1 2.97871 8.51988 -2 10 3 0 2.97871 8.51988 1 10 5 2 38.1328 3.82697 -2 -10 4 0 38.1328 3.82697 1 9 5 2 37.6625 7.75541 -2 -9 4 0 37.6625 7.75541 1 8 5 2 27.0802 4.05022 -2 -8 4 0 27.0802 4.05022 1 7 5 2 171.001 8.18541 -2 -7 4 0 171.001 8.18541 1 -6 4 0 47.8171 2.40966 1 -5 4 0 84.2684 3.06111 1 -4 4 0 271.595 6.46052 1 3 4 2 649.055 37.9040 -2 -3 4 0 649.055 37.9040 1 -2 4 0 405.006 7.75827 1 -1 4 0 19.6641 1.04724 1 0 4 0 -0.0992 0.60312 1 1 4 0 46.2455 1.61428 1 2 4 0 416.652 10.2144 1 3 4 0 394.345 8.95331 1 4 4 0 6.29258 1.75813 1 5 4 0 245.563 9.27544 1 6 4 0 9.20474 1.90021 1 7 4 0 52.6968 5.79179 1 8 4 0 31.3562 4.79411 1 9 4 0 101.953 5.12330 1 10 4 0 1.61409 2.36351 1 10 6 2 27.5953 6.49870 -2 -10 5 0 27.5953 6.49870 1 9 6 2 34.1675 4.07233 -2 -9 5 0 34.1675 4.07233 1 8 6 2 35.7531 7.15401 -2 -8 5 0 35.7531 7.15401 1 -7 5 0 -0.9327 1.34105 1 -6 5 0 13.1392 2.06253 1 -5 5 0 289.002 8.93053 1 4 5 2 269.671 11.6317 -2 -4 5 0 269.671 11.6317 1 3 5 2 322.289 9.17084 -2 -3 5 0 322.289 9.17084 1 2 5 2 37.2361 1.81982 -2 -2 5 0 37.2361 1.81982 1 1 5 2 233.500 6.13594 -2 -1 5 0 233.500 6.13594 1 0 5 2 865.116 29.0580 -2 0 5 0 865.116 29.0580 1 -1 5 2 13.4476 3.89270 -2 1 5 0 13.4476 3.89270 1 2 5 0 305.170 9.06774 1 3 5 0 30.7757 1.59357 1 -4 4 2 78.3538 11.5359 -2 4 5 0 78.3538 11.5359 1 -5 4 2 355.468 12.8773 -2 5 5 0 355.468 12.8773 1 -6 4 2 15.1757 2.81278 -2 6 5 0 15.1757 2.81278 1 -7 4 2 123.574 9.11904 -2 7 5 0 123.574 9.11904 1 -8 4 2 51.0249 5.58064 -2 8 5 0 51.0249 5.58064 1 -9 4 2 60.9290 6.56234 -2 9 5 0 60.9290 6.56234 1 -10 4 2 18.0946 8.01385 -2 10 5 0 18.0946 8.01385 1 10 7 3 -7.8106 8.49490 -2 -10 6 0 -7.8106 8.49490 1 9 7 3 15.0018 6.62074 -2 -9 6 0 15.0018 6.62074 1 8 7 3 12.2870 16.9045 -2 -8 6 0 12.2870 16.9045 1 -7 6 0 28.0944 2.94052 1 -6 6 0 59.5347 3.45178 1 -5 6 0 249.694 8.08094 1 -4 6 0 119.624 4.55807 1 -3 6 0 321.824 8.27738 1 -2 6 0 27.4632 1.95157 1 -1 6 0 121.085 3.24167 1 0 6 0 235.258 5.99045 1 1 6 0 117.997 3.23676 1 2 6 0 15.0942 1.52673 1 3 6 0 315.435 9.35967 1 4 6 0 37.9343 2.29889 1 -5 5 2 530.094 25.9932 -2 5 6 0 530.094 25.9932 1 -6 5 2 136.406 9.06782 -2 6 6 0 136.406 9.06782 1 7 6 0 1.48829 2.85670 1 -8 5 2 4.48100 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18.2959 -2 -4 8 0 202.768 18.2959 1 3 8 3 277.450 12.3600 -2 -3 8 0 277.450 12.3600 1 2 8 3 762.480 28.9003 -2 -2 8 0 762.480 28.9003 1 -1 8 0 333.090 11.2216 1 0 8 0 54.2201 3.56129 1 1 8 0 9.24904 1.84327 1 2 8 0 577.876 17.6535 1 3 8 0 5.73840 1.52800 1 -4 7 3 794.786 22.5463 -2 4 8 0 794.786 22.5463 1 -5 7 3 113.922 4.29835 -2 5 8 0 113.922 4.29835 1 -6 7 3 10.7085 3.02284 -2 6 8 0 10.7085 3.02284 1 -7 7 3 3.24487 2.97646 -2 7 8 0 3.24487 2.97646 1 -8 7 3 34.9563 7.17597 -2 8 8 0 34.9563 7.17597 1 -8 9 0 44.9370 5.25274 1 -7 9 0 8.91877 2.20282 1 6 9 4 2.62552 5.73897 -2 -6 9 0 2.62552 5.73897 1 5 9 4 149.775 7.30089 -2 -5 9 0 149.775 7.30089 1 4 9 4 39.0598 5.87152 -2 -4 9 0 39.0598 5.87152 1 3 9 4 335.524 14.8886 -2 -3 9 0 335.524 14.8886 1 2 9 4 40.0166 4.38127 -2 -2 9 0 40.0166 4.38127 1 -1 9 0 18.2715 2.20461 1 0 9 0 41.9640 3.36959 1 1 9 0 11.0342 2.03053 1 -2 8 4 21.6585 7.24314 -2 2 9 0 21.6585 7.24314 1 -3 8 4 26.4585 4.53662 -2 3 9 0 26.4585 4.53662 1 -4 8 4 40.8479 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0.82364 4.51505 -2 6 1 12 0.82364 4.51505 1 7 -3 11 64.6503 6.25477 -2 7 1 12 64.6503 6.25477 1 8 1 12 44.3195 4.52004 1 9 1 12 21.9078 3.19192 1 10 -2 11 10.9250 7.25287 -2 10 1 12 10.9250 7.25287 1 -1 2 12 8.92988 4.55640 1 0 2 12 4.78459 2.55589 1 1 2 12 68.9473 4.45063 1 2 -4 11 61.4666 12.2495 -2 2 2 12 61.4666 12.2495 1 3 -4 11 8.48961 7.95253 -2 3 2 12 8.48961 7.95253 1 4 -4 11 -10.051 7.50580 -2 4 2 12 -10.051 7.50580 1 5 -4 11 -1.5298 5.06881 -2 5 2 12 -1.5298 5.06881 1 6 -4 11 29.2763 6.46064 -2 6 2 12 29.2763 6.46064 1 7 -4 11 34.4577 6.68117 -2 7 2 12 34.4577 6.68117 1 8 2 12 26.2944 3.22956 1 9 2 12 12.9183 3.15625 1 10 -3 11 -13.049 7.45706 -2 10 2 12 -13.049 7.45706 1 -1 -6 10 -23.607 15.1910 -2 -1 3 12 -23.607 15.1910 1 0 3 12 -4.1699 2.38078 1 1 3 12 12.0248 2.71877 1 2 -5 10 36.7411 9.49376 -2 2 3 12 36.7411 9.49376 1 3 -5 10 5.00410 7.59903 -2 3 3 12 5.00410 7.59903 1 4 -5 10 49.5285 5.93980 -2 4 3 12 49.5285 5.93980 1 5 -5 10 19.1054 4.45597 -2 5 3 12 19.1054 4.45597 1 6 -5 10 38.9104 10.6966 -2 6 3 12 38.9104 10.6966 1 7 -5 10 40.6860 12.3266 -2 7 3 12 40.6860 12.3266 1 8 3 12 112.311 6.01779 1 9 3 12 0.75702 3.40254 1 10 3 12 -1.1973 3.51105 1 0 4 12 -2.0543 2.51325 1 1 -6 10 11.4887 8.32689 -2 1 4 12 11.4887 8.32689 1 2 -6 10 57.5049 5.47637 -2 2 4 12 57.5049 5.47637 1 3 -6 10 0.65179 4.19850 -2 3 4 12 0.65179 4.19850 1 4 -6 10 70.8951 6.03407 -2 4 4 12 70.8951 6.03407 1 5 -6 10 -0.7025 5.39556 -2 5 4 12 -0.7025 5.39556 1 6 -6 10 22.8012 6.32257 -2 6 4 12 22.8012 6.32257 1 7 4 12 -6.9518 2.61252 1 8 4 12 186.109 10.6499 1 9 -5 10 -2.8405 7.61569 -2 9 4 12 -2.8405 7.61569 1 0 5 12 -4.0862 2.39786 1 1 5 12 -0.0807 2.35812 1 2 5 12 0.39602 2.35548 1 3 -7 9 0.92574 11.1911 -2 3 5 12 0.92574 11.1911 1 4 -7 9 51.2038 11.3512 -2 4 5 12 51.2038 11.3512 1 5 -7 9 8.54846 18.3743 -2 5 5 12 8.54846 18.3743 1 6 5 12 10.8955 3.76941 1 7 5 12 13.8228 3.92528 1 8 5 12 47.2678 5.46844 1 9 5 12 8.42884 3.58236 1 1 -8 9 3.08855 4.75370 -2 1 6 12 3.08855 4.75370 1 2 -8 9 76.8192 4.78480 -2 2 6 12 76.8192 4.78480 1 3 -8 9 30.0315 4.32651 -2 3 6 12 30.0315 4.32651 1 4 -8 9 170.328 8.18313 -2 4 6 12 170.328 8.18313 1 5 -8 9 -8.7006 9.96571 -2 5 6 12 -8.7006 9.96571 1 6 -8 9 7.08615 7.95840 -2 6 6 12 7.08615 7.95840 1 7 6 12 -2.1071 3.24285 1 8 -7 9 74.7145 9.29634 -2 8 6 12 74.7145 9.29634 1 2 7 12 14.2908 3.15042 1 3 7 12 12.4483 3.65721 1 4 7 12 -5.6108 4.75980 1 5 7 12 -4.6147 4.84503 1 6 7 12 21.2815 3.70639 1 7 7 12 -7.6367 2.99051 1 4 -10 8 36.6530 18.5027 -2 4 8 12 36.6530 18.5027 1 5 8 12 56.4865 7.05908 1 4 -3 13 43.7230 3.31549 1 5 1 14 -11.266 11.9950 -2 5 -3 13 -11.266 11.9950 1 6 1 14 61.0205 6.54445 -2 6 -3 13 61.0205 6.54445 1 7 -3 13 18.8838 3.25471 1 2 -1 13 43.7969 8.74163 -2 2 -2 13 43.7969 8.74163 1 3 -2 13 83.5204 4.67590 1 4 -2 13 20.5691 3.05359 1 5 -2 13 34.2116 3.46438 1 6 -2 13 -2.1097 2.06127 1 7 -2 13 1.39761 2.91586 1 8 -2 13 30.5926 4.49423 1 2 -1 13 32.0857 3.22849 1 3 -1 13 8.50296 3.21407 1 4 -1 13 1.87634 1.81308 1 5 -1 13 -0.1128 4.82693 -2 5 -1 13 -0.1128 4.82693 1 6 -1 13 100.143 9.01309 -2 6 -1 13 100.143 9.01309 1 7 -1 13 -5.1939 5.34371 -2 7 -1 13 -5.1939 5.34371 1 8 -1 13 28.0584 4.05323 -2 8 -1 13 28.0584 4.05323 1 1 0 13 -1.3892 2.70104 1 2 0 13 1.13068 3.37647 1 3 0 13 69.7047 3.77609 1 4 0 13 0.82435 2.39801 1 5 0 13 72.2669 4.74642 1 6 0 13 3.86988 2.52919 1 7 0 13 1.83235 1.93197 1 8 0 13 11.8362 2.93501 1 9 0 13 17.8642 3.15994 1 1 1 13 10.4367 2.92570 1 2 1 13 17.8719 3.96371 1 3 1 13 8.98136 2.15079 1 4 -3 12 6.05482 8.03244 -2 4 1 13 6.05482 8.03244 1 5 -3 12 7.76352 5.04560 -2 5 1 13 7.76352 5.04560 1 6 -3 12 15.9016 3.51353 -2 6 1 13 15.9016 3.51353 1 7 -3 12 -9.9937 5.53340 -2 7 1 13 -9.9937 5.53340 1 8 -3 12 43.8191 5.34856 -2 8 1 13 43.8191 5.34856 1 9 -3 12 8.12868 6.57969 -2 9 1 13 8.12868 6.57969 1 1 2 13 42.9347 4.53556 1 2 2 13 19.6646 3.01640 1 3 2 13 -1.1913 2.61731 1 4 -4 12 71.0590 17.1713 -2 4 2 13 71.0590 17.1713 1 5 -4 12 17.3169 5.55946 -2 5 2 13 17.3169 5.55946 1 6 -4 12 168.573 8.75446 -2 6 2 13 168.573 8.75446 1 7 -4 12 45.4395 6.61336 -2 7 2 13 45.4395 6.61336 1 8 2 13 25.9395 5.24304 1 9 2 13 4.47319 3.61826 1 1 3 13 23.9061 4.96533 1 2 3 13 -1.3850 2.61884 1 3 3 13 22.0889 3.49580 1 4 -5 11 7.66024 8.28575 -2 4 3 13 7.66024 8.28575 1 5 -5 11 15.3426 8.23206 -2 5 3 13 15.3426 8.23206 1 6 -5 11 20.7144 4.99548 -2 6 3 13 20.7144 4.99548 1 7 -5 11 -4.3669 6.99059 -2 7 3 13 -4.3669 6.99059 1 8 3 13 10.0958 3.74174 1 9 3 13 61.7684 6.40041 1 2 4 13 83.8156 5.86410 1 3 -6 11 24.7595 6.97023 -2 3 4 13 24.7595 6.97023 1 4 -6 11 21.3330 5.23196 -2 4 4 13 21.3330 5.23196 1 5 -6 11 13.4973 7.52832 -2 5 4 13 13.4973 7.52832 1 6 -6 11 102.009 7.24183 -2 6 4 13 102.009 7.24183 1 7 -6 11 -0.0444 6.73342 -2 7 4 13 -0.0444 6.73342 1 8 4 13 66.0044 13.4949 1 2 5 13 6.54186 2.70700 1 3 5 13 45.1925 4.18095 1 4 5 13 3.76090 2.89493 1 5 -7 10 24.9513 12.4300 -2 5 5 13 24.9513 12.4300 1 6 5 13 4.98408 3.41521 1 7 5 13 1.33222 3.09424 1 4 -8 10 15.5822 4.62277 -2 4 6 13 15.5822 4.62277 1 5 -8 10 -7.4879 12.4816 -2 5 6 13 -7.4879 12.4816 1 6 -8 10 -29.401 16.1454 -2 6 6 13 -29.401 16.1454 1 5 1 14 25.1964 3.65504 1 6 -3 13 20.2575 6.55408 -2 6 1 14 20.2575 6.55408 1 5 2 14 8.92797 3.07299 1 6 2 14 20.3304 2.98173 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 66501 _shelx_res_file ; TITL PicTh35_0m_4_b.res in P-1 PicTh35_0m_5.res created by SHELXL-2019/1 at 12:02:21 on 04-Sep-2023 CELL 0.71073 10.0356 10.6643 11.2760 83.540 64.178 89.593 ZERR 4.00 0.0035 0.0033 0.0040 0.009 0.009 0.009 LATT 1 SFAC C O F S H UNIT 16 24 24 8 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 L.S. 5 FMAP 2 ACTA PLAN 10 WGHT 0.035600 5.679400 BASF 0.37272 FVAR 0.51437 C1 1 0.738964 0.780569 -0.314510 11.00000 0.02644 0.03238 = 0.03350 -0.00424 -0.01371 -0.00045 C2 1 0.798102 0.542623 -0.095187 11.00000 0.03775 0.01760 = 0.05517 -0.01243 -0.02917 0.01095 AFIX 23 H2A 5 0.902806 0.520173 -0.141213 11.00000 -1.20000 H2B 5 0.739825 0.497232 -0.130181 11.00000 -1.20000 AFIX 0 C3 1 0.740760 0.503776 0.050529 11.00000 0.02828 0.01717 = 0.04602 -0.00538 -0.02573 0.00024 AFIX 23 H3A 5 0.642752 0.539256 0.098399 11.00000 -1.20000 H3B 5 0.728878 0.410543 0.069459 11.00000 -1.20000 AFIX 0 C4 1 0.703061 0.580681 0.348086 11.00000 0.04695 0.03241 = 0.03605 -0.00241 -0.02517 -0.00033 C5 1 0.858927 0.272599 0.625711 11.00000 0.03646 0.02363 = 0.03244 -0.00486 -0.01668 0.00569 C6 1 0.792749 0.099816 0.913818 11.00000 0.01936 0.01580 = 0.03402 -0.00097 -0.01475 0.00320 AFIX 23 H6A 5 0.899447 0.113447 0.889450 11.00000 -1.20000 H6B 5 0.782152 0.034746 0.862035 11.00000 -1.20000 AFIX 0 C7 1 0.711141 0.056400 1.057814 11.00000 0.02104 0.02380 = 0.03210 -0.00106 -0.01640 -0.00049 AFIX 23 H7A 5 0.753362 -0.021922 1.080005 11.00000 -1.20000 H7B 5 0.605728 0.037346 1.080766 11.00000 -1.20000 AFIX 0 C8 1 0.739035 0.066060 1.353370 11.00000 0.03915 0.03727 = 0.03519 -0.00476 -0.02019 -0.00152 O1 2 0.541628 0.637430 -0.111455 11.00000 0.02277 0.02093 = 0.05101 -0.00499 -0.01650 -0.00506 O2 2 0.615607 0.846998 -0.077976 11.00000 0.02673 0.01912 = 0.03507 -0.00482 -0.01035 0.00146 O3 2 0.786947 0.680016 -0.120796 11.00000 0.02624 0.02310 = 0.03782 -0.00242 -0.01930 0.00376 O4 2 0.847447 0.551171 0.096084 11.00000 0.02453 0.02159 = 0.04223 0.00033 -0.02200 0.00044 O5 2 0.714816 0.746732 0.154609 11.00000 0.03061 0.01918 = 0.04286 -0.00153 -0.02106 0.00544 O6 2 0.948096 0.701962 0.175925 11.00000 0.03238 0.03362 = 0.05649 0.00185 -0.02929 -0.01087 O7 2 0.626491 0.119242 0.753681 11.00000 0.03353 0.02235 = 0.04901 -0.00547 -0.02556 -0.00205 O8 2 0.602259 0.347753 0.786102 11.00000 0.02834 0.02142 = 0.04250 -0.00559 -0.01906 0.00856 O9 2 0.732330 0.218645 0.882920 11.00000 0.02174 0.01647 = 0.02846 -0.00339 -0.01136 0.00271 O10 2 0.722195 0.156100 1.135954 11.00000 0.02928 0.02468 = 0.03560 -0.00705 -0.02174 0.00924 O11 2 0.960769 0.079483 1.118966 11.00000 0.02430 0.03408 = 0.04368 -0.01108 -0.01890 0.00982 O12 2 0.861763 0.277606 1.211804 11.00000 0.03961 0.02570 = 0.04635 -0.00397 -0.02282 0.00453 F1 3 0.795633 0.681574 -0.379229 11.00000 0.05538 0.04812 = 0.03609 -0.01490 -0.01785 0.00755 F2 3 0.638310 0.827313 -0.353268 11.00000 0.05701 0.05893 = 0.04461 -0.00245 -0.03509 0.01271 F3 3 0.846727 0.868661 -0.348409 11.00000 0.04319 0.03734 = 0.03793 0.00694 -0.00774 -0.01087 F4 3 0.590843 0.512900 0.350265 11.00000 0.04664 0.05483 = 0.03748 0.00944 -0.01237 -0.02306 F5 3 0.784093 0.505067 0.385517 11.00000 0.06723 0.03557 = 0.05332 0.01243 -0.03447 -0.00153 F6 3 0.648565 0.664162 0.432046 11.00000 0.07154 0.04858 = 0.04166 -0.00744 -0.01968 0.00546 F7 3 0.838874 0.281918 0.515655 11.00000 0.05481 0.04012 = 0.02584 -0.00210 -0.01974 0.00101 F8 3 0.918982 0.380531 0.629962 11.00000 0.03360 0.03347 = 0.03597 -0.00106 -0.01198 -0.00975 F9 3 0.952081 0.181989 0.620240 11.00000 0.03030 0.03619 = 0.03239 -0.00034 -0.00558 0.01251 F10 3 0.686141 -0.044923 1.341981 11.00000 0.09099 0.04006 = 0.03973 0.01031 -0.02862 -0.03045 F11 3 0.626457 0.126950 1.430040 11.00000 0.03950 0.07195 = 0.03529 -0.00894 -0.00768 -0.00082 F12 3 0.827603 0.042770 1.411019 11.00000 0.07203 0.03818 = 0.04453 0.00634 -0.03792 -0.00105 S1 4 0.651292 0.733510 -0.137093 11.00000 0.01960 0.01745 = 0.02663 -0.00135 -0.01062 0.00050 S2 4 0.811475 0.661629 0.180554 11.00000 0.02575 0.01930 = 0.03299 0.00124 -0.01734 -0.00255 S3 4 0.681159 0.234931 0.770889 11.00000 0.02058 0.01884 = 0.03167 -0.00242 -0.01448 0.00192 S4 4 0.840457 0.153609 1.189724 11.00000 0.02513 0.01843 = 0.03010 -0.00130 -0.01473 0.00302 HKLF 5 1 1 0 0 0 1 0 0 0 1 REM PicTh35_0m_4_b.res in P-1 REM wR2 = 0.1657, GooF = S = 1.073, Restrained GooF = 1.073 for all data REM R1 = 0.0658 for 3403 Fo > 4sig(Fo) and 0.0941 for all 4339 data REM 326 parameters refined using 0 restraints END WGHT 0.0356 5.6795 REM Highest difference peak 0.604, deepest hole -0.548, 1-sigma level 0.128 Q1 1 0.6913 0.7403 -0.2330 11.00000 0.05 0.60 Q2 1 0.7594 0.2640 0.6598 11.00000 0.05 0.57 Q3 1 0.7770 0.1274 1.2848 11.00000 0.05 0.55 Q4 1 0.7472 0.6593 0.2908 11.00000 0.05 0.55 Q5 1 1.0329 0.0933 1.0007 11.00000 0.05 0.54 Q6 1 0.8780 0.6803 0.0650 11.00000 0.05 0.53 Q7 1 0.9406 0.5341 0.1116 11.00000 0.05 0.52 Q8 1 0.6586 0.1990 1.3829 11.00000 0.05 0.50 Q9 1 0.5859 0.7172 0.0008 11.00000 0.05 0.49 Q10 1 0.7013 0.3941 0.6897 11.00000 0.05 0.49 ; _shelx_res_checksum 42524 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.7390(7) 0.7806(7) -0.3145(7) 0.0305(15) Uani d 1 . . C C2 0.7981(8) 0.5426(6) -0.0952(8) 0.0330(16) Uani d 1 . . H H2A 0.902806 0.520173 -0.141213 0.040 Uiso calc 1 . . H H2B 0.739825 0.497232 -0.130181 0.040 Uiso calc 1 . . C C3 0.7408(7) 0.5038(6) 0.0505(7) 0.0269(14) Uani d 1 . . H H3A 0.642752 0.539256 0.098399 0.032 Uiso calc 1 . . H H3B 0.728878 0.410543 0.069459 0.032 Uiso calc 1 . . C C4 0.7031(9) 0.5807(7) 0.3481(7) 0.0361(17) Uani d 1 . . C C5 0.8589(8) 0.2726(6) 0.6257(7) 0.0302(14) Uani d 1 . . C C6 0.7927(7) 0.0998(5) 0.9138(6) 0.0221(13) Uani d 1 . . H H6A 0.899447 0.113447 0.889450 0.027 Uiso calc 1 . . H H6B 0.782152 0.034746 0.862035 0.027 Uiso calc 1 . . C C7 0.7111(7) 0.0564(6) 1.0578(6) 0.0241(13) Uani d 1 . . H H7A 0.753362 -0.021922 1.080005 0.029 Uiso calc 1 . . H H7B 0.605728 0.037346 1.080766 0.029 Uiso calc 1 . . C C8 0.7390(8) 0.0661(7) 1.3534(7) 0.0357(17) Uani d 1 . . O O1 0.5416(5) 0.6374(4) -0.1115(5) 0.0314(11) Uani d 1 . . O O2 0.6156(5) 0.8470(4) -0.0780(5) 0.0280(10) Uani d 1 . . O O3 0.7869(5) 0.6800(4) -0.1208(5) 0.0273(10) Uani d 1 . . O O4 0.8474(5) 0.5512(4) 0.0961(5) 0.0271(10) Uani d 1 . . O O5 0.7148(5) 0.7467(4) 0.1546(5) 0.0293(10) Uani d 1 . . O O6 0.9481(5) 0.7020(5) 0.1759(5) 0.0378(12) Uani d 1 . . O O7 0.6265(5) 0.1192(4) 0.7537(5) 0.0321(11) Uani d 1 . . O O8 0.6023(5) 0.3478(4) 0.7861(5) 0.0294(10) Uani d 1 . . O O9 0.7323(4) 0.2186(4) 0.8829(4) 0.0220(9) Uani d 1 . . O O10 0.7222(5) 0.1561(4) 1.1360(4) 0.0269(10) Uani d 1 . . O O11 0.9608(5) 0.0795(4) 1.1190(5) 0.0321(11) Uani d 1 . . O O12 0.8618(5) 0.2776(4) 1.2118(5) 0.0358(12) Uani d 1 . . F F1 0.7956(5) 0.6816(4) -0.3792(4) 0.0465(11) Uani d 1 . . F F2 0.6383(5) 0.8273(4) -0.3533(5) 0.0492(12) Uani d 1 . . F F3 0.8467(5) 0.8687(4) -0.3484(4) 0.0440(11) Uani d 1 . . F F4 0.5908(5) 0.5129(4) 0.3503(4) 0.0496(12) Uani d 1 . . F F5 0.7841(6) 0.5051(4) 0.3855(5) 0.0506(12) Uani d 1 . . F F6 0.6486(6) 0.6642(5) 0.4320(5) 0.0556(13) Uani d 1 . . F F7 0.8389(5) 0.2819(4) 0.5157(4) 0.0397(10) Uani d 1 . . F F8 0.9190(4) 0.3805(4) 0.6300(4) 0.0357(9) Uani d 1 . . F F9 0.9521(4) 0.1820(4) 0.6202(4) 0.0363(10) Uani d 1 . . F F10 0.6861(6) -0.0449(4) 1.3420(5) 0.0580(14) Uani d 1 . . F F11 0.6265(5) 0.1269(5) 1.4300(4) 0.0518(12) Uani d 1 . . F F12 0.8276(6) 0.0428(4) 1.4110(4) 0.0480(12) Uani d 1 . . S S1 0.65129(17) 0.73351(14) -0.13709(15) 0.0212(3) Uani d 1 . . S S2 0.81148(18) 0.66163(14) 0.18055(17) 0.0247(4) Uani d 1 . . S S3 0.68116(17) 0.23493(14) 0.77089(16) 0.0227(3) Uani d 1 . . S S4 0.84046(18) 0.15361(14) 1.18972(16) 0.0237(3) 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 0.026(4) 0.032(4) 0.033(4) 0.000(3) -0.014(3) -0.004(3) C2 0.038(4) 0.018(3) 0.055(5) 0.011(3) -0.029(4) -0.012(3) C3 0.028(3) 0.017(3) 0.046(4) 0.000(2) -0.026(3) -0.005(3) C4 0.047(4) 0.032(4) 0.036(4) 0.000(3) -0.025(4) -0.002(3) C5 0.036(4) 0.024(3) 0.032(4) 0.006(3) -0.017(3) -0.005(3) C6 0.019(3) 0.016(3) 0.034(4) 0.003(2) -0.015(3) -0.001(2) C7 0.021(3) 0.024(3) 0.032(3) 0.000(3) -0.016(3) -0.001(3) C8 0.039(4) 0.037(4) 0.035(4) -0.002(3) -0.020(4) -0.005(3) O1 0.023(2) 0.021(2) 0.051(3) -0.0051(18) -0.016(2) -0.005(2) O2 0.027(2) 0.019(2) 0.035(3) 0.0015(18) -0.010(2) -0.0048(19) O3 0.026(2) 0.023(2) 0.038(3) 0.0038(18) -0.019(2) -0.0024(19) O4 0.025(2) 0.022(2) 0.042(3) 0.0004(17) -0.022(2) 0.0003(19) O5 0.031(3) 0.019(2) 0.043(3) 0.0054(18) -0.021(2) -0.0015(19) O6 0.032(3) 0.034(3) 0.056(3) -0.011(2) -0.029(3) 0.002(2) O7 0.034(3) 0.022(2) 0.049(3) -0.0020(19) -0.026(2) -0.005(2) O8 0.028(2) 0.021(2) 0.042(3) 0.0086(18) -0.019(2) -0.0056(19) O9 0.022(2) 0.016(2) 0.028(2) 0.0027(16) -0.0114(19) -0.0034(17) O10 0.029(2) 0.025(2) 0.036(3) 0.0092(18) -0.022(2) -0.0071(19) O11 0.024(2) 0.034(3) 0.044(3) 0.0098(19) -0.019(2) -0.011(2) O12 0.040(3) 0.026(2) 0.046(3) 0.005(2) -0.023(3) -0.004(2) F1 0.055(3) 0.048(3) 0.036(2) 0.008(2) -0.018(2) -0.015(2) F2 0.057(3) 0.059(3) 0.045(3) 0.013(2) -0.035(2) -0.002(2) F3 0.043(3) 0.037(2) 0.038(2) -0.0109(19) -0.008(2) 0.0069(19) F4 0.047(3) 0.055(3) 0.037(2) -0.023(2) -0.012(2) 0.009(2) F5 0.067(3) 0.036(2) 0.053(3) -0.002(2) -0.034(3) 0.012(2) F6 0.072(3) 0.049(3) 0.042(3) 0.005(2) -0.020(3) -0.007(2) F7 0.055(3) 0.040(2) 0.026(2) 0.001(2) -0.020(2) -0.0021(17) F8 0.034(2) 0.033(2) 0.036(2) -0.0097(17) -0.0120(19) -0.0011(17) F9 0.030(2) 0.036(2) 0.032(2) 0.0125(17) -0.0056(18) -0.0003(17) F10 0.091(4) 0.040(3) 0.040(3) -0.030(3) -0.029(3) 0.010(2) F11 0.040(3) 0.072(3) 0.035(2) -0.001(2) -0.008(2) -0.009(2) F12 0.072(3) 0.038(3) 0.045(3) -0.001(2) -0.038(3) 0.006(2) S1 0.0196(7) 0.0175(7) 0.0266(8) 0.0005(6) -0.0106(6) -0.0014(6) S2 0.0257(8) 0.0193(7) 0.0330(9) -0.0026(6) -0.0173(7) 0.0012(6) S3 0.0206(7) 0.0188(7) 0.0317(8) 0.0019(6) -0.0145(7) -0.0024(6) S4 0.0251(8) 0.0184(7) 0.0301(8) 0.0030(6) -0.0147(7) -0.0013(6) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag F3 C1 F1 . . 108.8(6) ? F3 C1 F2 . . 108.5(6) ? F1 C1 F2 . . 107.9(6) ? F3 C1 S1 . . 111.3(5) ? F1 C1 S1 . . 110.6(5) ? F2 C1 S1 . . 109.6(5) ? O3 C2 C3 . . 109.8(5) ? O4 C3 C2 . . 108.9(5) ? F5 C4 F6 . . 109.2(6) ? F5 C4 F4 . . 108.6(6) ? F6 C4 F4 . . 108.5(7) ? F5 C4 S2 . . 111.3(5) ? F6 C4 S2 . . 109.7(5) ? F4 C4 S2 . . 109.5(5) ? F8 C5 F9 . . 108.6(6) ? F8 C5 F7 . . 108.5(5) ? F9 C5 F7 . . 108.8(6) ? F8 C5 S3 . . 111.2(5) ? F9 C5 S3 . . 110.0(4) ? F7 C5 S3 . . 109.6(5) ? O9 C6 C7 . . 109.1(5) ? C6 C7 O10 . . 110.0(5) ? F11 C8 F12 . . 108.9(6) ? F11 C8 F10 . . 107.7(6) ? F12 C8 F10 . . 108.1(6) ? F11 C8 S4 . . 112.1(5) ? F12 C8 S4 . . 110.2(5) ? F10 C8 S4 . . 109.6(5) ? C2 O3 S1 . . 120.5(4) ? C3 O4 S2 . . 121.4(4) ? C6 O9 S3 . . 121.4(4) ? C7 O10 S4 . . 121.4(4) ? O2 S1 O1 . . 121.9(3) ? O2 S1 O3 . . 108.4(3) ? O1 S1 O3 . . 112.0(3) ? O2 S1 C1 . . 105.9(3) ? O1 S1 C1 . . 107.1(3) ? O3 S1 C1 . . 98.9(3) ? O6 S2 O5 . . 122.7(3) ? O6 S2 O4 . . 105.6(3) ? O5 S2 O4 . . 112.3(3) ? O6 S2 C4 . . 106.2(3) ? O5 S2 C4 . . 106.0(3) ? O4 S2 C4 . . 101.8(3) ? O7 S3 O8 . . 123.2(3) ? O7 S3 O9 . . 112.2(3) ? O8 S3 O9 . . 106.4(3) ? O7 S3 C5 . . 106.0(3) ? O8 S3 C5 . . 105.9(3) ? O9 S3 C5 . . 100.5(3) ? O12 S4 O11 . . 122.1(3) ? O12 S4 O10 . . 107.5(3) ? O11 S4 O10 . . 111.9(3) ? O12 S4 C8 . . 105.7(3) ? O11 S4 C8 . . 106.3(3) ? O10 S4 C8 . . 101.1(3) ? 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 F3 . 1.331(8) ? C1 F1 . 1.332(8) ? C1 F2 . 1.337(8) ? C1 S1 . 1.810(7) ? C2 O3 . 1.474(7) ? C2 C3 . 1.493(10) ? C3 O4 . 1.487(7) ? C4 F5 . 1.305(8) ? C4 F6 . 1.311(9) ? C4 F4 . 1.332(8) ? C4 S2 . 1.831(8) ? C5 F8 . 1.318(8) ? C5 F9 . 1.327(8) ? C5 F7 . 1.334(8) ? C5 S3 . 1.828(7) ? C6 O9 . 1.473(7) ? C6 C7 . 1.483(9) ? C7 O10 . 1.489(7) ? C8 F11 . 1.308(9) ? C8 F12 . 1.318(8) ? C8 F10 . 1.342(8) ? C8 S4 . 1.817(8) ? O1 S1 . 1.420(4) ? O2 S1 . 1.416(4) ? O3 S1 . 1.548(4) ? O4 S2 . 1.540(5) ? O5 S2 . 1.423(4) ? O6 S2 . 1.417(5) ? O7 S3 . 1.420(4) ? O8 S3 . 1.421(4) ? O9 S3 . 1.551(4) ? O10 S4 . 1.549(4) ? O11 S4 . 1.417(5) ? O12 S4 . 1.407(5) ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F5 F7 2.823(7) 1_555 1_555 yes F7 F12 2.951(7) 1_555 1_554 yes F3 F9 2.954(5) 1_555 2_765 yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _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 C2 H2B O8 1_555 1_555 1_554 0.99 2.615 3.600(10) 171.72 yes C3 H3A O1 1_555 1_555 2_665 0.99 2.597 2.984(9) 103.25 yes C3 H3B O1 1_555 1_555 2_665 0.99 2.588 2.984(9) 103.80 yes C3 H3A O8 1_555 1_555 2_666 0.99 2.591 3.579(8) 174.78 yes C6 H6A O6 1_555 1_555 2_766 0.99 2.343 3.092(8) 131.72 yes C6 H6A O11 1_555 1_555 2_757 0.99 2.469 3.034(8) 115.81 yes C6 H6B O2 1_555 1_555 1_564 0.99 2.453 3.210(8) 132.93 yes C7 H7A O5 1_555 1_555 1_564 0.99 2.492 3.365(8) 146.89 yes C7 H7B O7 1_555 1_555 2_657 0.99 2.696 3.525(7) 141.55 yes C7 H7B O2 1_555 1_555 2_666 0.99 2.543 3.349(9) 138.49 yes