#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:52:58 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253999 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240483.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7240483 loop_ _publ_author_name 'Rabideau, Brooks D.' 'Soltani, Mohammad' 'Parker, Rome A.' 'Siu, Benjamin' 'Salter, E. Alan' 'Wierzbicki, Andrzej' 'West, Kevin N.' 'Davis, Jr, James H' _publ_section_title ; Tuning the melting point of selected ionic liquids through adjustment of the cation's dipole moment. ; _journal_issue 21 _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_page_first 12301 _journal_page_last 12311 _journal_paper_doi 10.1039/d0cp01214a _journal_volume 22 _journal_year 2020 _chemical_formula_moiety 'C30 H23 F O P, C2 F6 N O4 S2' _chemical_formula_sum 'C32 H23 F7 N O5 P S2' _chemical_formula_weight 729.60 _chemical_name_systematic '[4-(2-fluorphenoxy)phenyl]triphenylphosphonium bistriflimide' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-02-25 deposited with the CCDC. 2020-05-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 18.0015(14) _cell_length_b 18.7263(15) _cell_length_c 18.8837(16) _cell_measurement_reflns_used 9810 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 33.1353 _cell_measurement_theta_min 2.4313 _cell_volume 6365.7(9) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2016)' _computing_data_collection 'Apex3 v2018.1-0 (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2016)' _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2015, 2018), SHELXLE Rev946 (H\"ubschle et al., 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker AXS D8 Quest CMOS diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'Triumph curved graphite crystal' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_unetI/netI 0.0229 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 147999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.230 _diffrn_reflns_theta_min 2.157 _diffrn_source 'fine focus sealed tube X-ray source' _diffrn_source_current '30 mA' _diffrn_source_voltage '50 kV' _exptl_absorpt_coefficient_mu 0.301 _exptl_absorpt_correction_T_max 0.7465 _exptl_absorpt_correction_T_min 0.6890 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.523 _exptl_crystal_description plate _exptl_crystal_F_000 2976 _exptl_crystal_size_max 0.520 _exptl_crystal_size_mid 0.460 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.790 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 579 _refine_ls_number_reflns 12152 _refine_ls_number_restraints 513 _refine_ls_restrained_S_all 1.127 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0579 _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^)+(0.0967P)^2^+4.2261P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1578 _refine_ls_wR_factor_ref 0.1854 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8861 _reflns_number_total 12152 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cp01214a2.cif _cod_data_source_block JD_POP_OF_0m _cod_depositor_comments 'Adding full bibliography for 7240483--7240486.cif.' _cod_database_code 7240483 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.859 _shelx_estimated_absorpt_t_max 0.939 _shelx_res_file ; TITL JD_POP_OF_0m in Pbca JD_POP_OF_0m.res created by SHELXL-2018/3 at 18:22:00 on 15-Mar-2019 CELL 0.71073 18.00150 18.72630 18.88370 90.0000 90.0000 90.0000 ZERR 8.00 0.00140 0.00150 0.00160 0.0000 0.0000 0.0000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N O F P S UNIT 256 184 8 40 56 8 16 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.120 SIZE 0.21 0.46 0.52 L.S. 14 BOND $H ACTA FMAP 2 REM TWIN 0 1 0 1 0 0 0 0 -1 PLAN 120 REM DAMP 200 SIMU 0.01 0.01 F2 > O5B WGHT 0.096700 4.226100 FVAR 0.27543 0.68262 0.84560 PART 1 31 F2 5 0.910524 0.066425 0.800559 31.00000 0.05579 0.07839 = 0.03949 0.00174 0.00223 0.00111 F3 5 0.990033 -0.010419 0.763453 31.00000 0.08288 0.10189 = 0.08393 0.02098 -0.01503 0.05178 F4 5 1.000427 0.102072 0.734728 31.00000 0.04497 0.10236 = 0.05975 0.00098 -0.00827 -0.02515 C31 1 0.952986 0.048867 0.745746 31.00000 0.03433 0.05954 = 0.04567 0.01176 -0.00181 0.00821 S1 7 0.897222 0.030313 0.666739 31.00000 0.03543 0.03082 = 0.04143 -0.00219 0.00453 0.00110 O2 4 0.842023 -0.019385 0.692616 31.00000 0.05305 0.03074 = 0.06808 0.00361 0.00843 -0.00819 O3 4 0.949140 0.006605 0.614763 31.00000 0.05811 0.05109 = 0.05927 -0.01200 0.01859 0.00905 N1 3 0.857244 0.104015 0.652961 31.00000 0.03182 0.03819 = 0.04066 0.00891 0.00477 0.00094 F5 5 0.760995 0.152347 0.537203 31.00000 0.06100 0.16002 = 0.10119 0.05151 -0.04243 -0.03393 F6 5 0.847312 0.092681 0.494694 31.00000 0.18259 0.11973 = 0.06522 -0.04322 -0.02793 -0.03363 F7 5 0.846377 0.207452 0.480275 31.00000 0.11315 0.13819 = 0.05960 0.05414 -0.01899 -0.03118 C32 1 0.833274 0.153613 0.524630 31.00000 0.07462 0.08646 = 0.04046 0.01242 -0.01760 -0.02702 S2 7 0.886671 0.166276 0.604719 31.00000 0.03218 0.03104 = 0.02940 -0.00145 -0.00076 -0.00439 O4 4 0.860545 0.233380 0.630943 31.00000 0.08484 0.03591 = 0.06334 -0.00853 0.01997 -0.00351 O5 4 0.962087 0.162547 0.582703 31.00000 0.03230 0.06000 = 0.06852 0.01800 0.00663 -0.00764 PART 2 -31 SAME F2 > O5 F2B 5 0.915117 0.104061 0.781222 -31.00000 0.06491 0.08244 = 0.04942 -0.00574 -0.00036 0.00617 F3B 5 0.945603 -0.006571 0.793193 -31.00000 0.07571 0.08826 = 0.07417 0.02355 -0.00874 0.00920 F4B 5 1.026120 0.059690 0.748302 -31.00000 0.04993 0.09621 = 0.06939 0.01586 -0.00638 -0.00927 C31B 1 0.953476 0.050712 0.753002 -31.00000 0.05226 0.07296 = 0.05583 0.00947 -0.00531 0.00450 S1B 7 0.916646 0.028319 0.665100 -31.00000 0.04715 0.03192 = 0.06257 0.00954 0.00322 0.00034 O2B 4 0.841601 0.010983 0.679286 -31.00000 0.04307 0.04581 = 0.05863 0.00434 0.00488 -0.01240 O3B 4 0.966202 -0.025187 0.639119 -31.00000 0.06217 0.04326 = 0.06951 0.00197 0.01670 0.01029 N1B 3 0.933243 0.105352 0.632691 -31.00000 0.04438 0.04409 = 0.05247 0.00720 -0.00349 -0.00430 F5B 5 0.773356 0.143977 0.599168 -31.00000 0.07446 0.09929 = 0.08019 0.01254 0.00036 -0.01238 F6B 5 0.827104 0.227797 0.613025 -31.00000 0.08416 0.06634 = 0.07434 -0.00903 0.00108 -0.00050 F7B 5 0.802971 0.203845 0.502779 -31.00000 0.08773 0.12164 = 0.06937 0.03387 -0.03005 -0.01494 C32B 1 0.825905 0.179767 0.564252 -31.00000 0.07195 0.08622 = 0.05895 0.01324 -0.01041 -0.01748 S2B 7 0.905990 0.124974 0.559710 -31.00000 0.05331 0.05097 = 0.04005 -0.00260 -0.00437 -0.00627 O4B 4 0.889650 0.076219 0.505998 -31.00000 0.08766 0.08294 = 0.04644 -0.03780 -0.01668 0.00387 O5B 4 0.962709 0.172033 0.527839 -31.00000 0.05967 0.07567 = 0.06675 0.00935 0.00397 -0.00804 PART 0 P1 6 0.681595 0.252537 0.278734 11.00000 0.02169 0.02103 = 0.02321 0.00263 0.00141 -0.00138 PART 1 F1 5 0.419031 0.146680 0.548257 21.00000 0.05279 0.07757 = 0.07754 -0.04019 -0.00645 -0.01784 PART 2 F1B 5 0.429284 -0.013211 0.372753 -21.00000 0.04928 0.05116 = 0.04830 -0.01416 0.00765 0.00356 PART 0 O1 4 0.502130 0.064327 0.464168 11.00000 0.02451 0.04720 = 0.04674 0.02604 -0.00058 -0.00729 C1 1 0.425130 0.063506 0.460146 11.00000 0.02504 0.03802 = 0.04169 0.01524 0.00203 -0.00632 C2 1 0.383434 0.104031 0.505566 11.00000 0.03494 0.05170 = 0.05605 -0.00660 0.00228 -0.01183 PART 2 -21 AFIX 43 H2 2 0.407767 0.134820 0.538133 -21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.306884 0.101123 0.505064 11.00000 0.03583 0.06659 = 0.06725 -0.01809 0.01264 -0.00566 AFIX 43 H3 2 0.278937 0.129449 0.537189 11.00000 -1.20000 AFIX 0 C4 1 0.271165 0.056918 0.457725 11.00000 0.02619 0.05851 = 0.05477 0.00195 0.00355 -0.00861 AFIX 43 H4 2 0.218432 0.055249 0.456653 11.00000 -1.20000 AFIX 0 C5 1 0.311982 0.015058 0.411857 11.00000 0.03435 0.04858 = 0.04103 0.00527 -0.00246 -0.01106 AFIX 43 H5 2 0.287665 -0.015876 0.379416 11.00000 -1.20000 AFIX 0 C6 1 0.389096 0.018680 0.413672 11.00000 0.03237 0.04455 = 0.03738 0.00957 0.00337 -0.00254 PART 1 21 AFIX 43 H6 2 0.417379 -0.010238 0.382343 21.00000 -1.20000 AFIX 0 PART 0 C7 1 0.540580 0.107826 0.418715 11.00000 0.02288 0.02737 = 0.02639 0.00583 -0.00107 -0.00524 C8 1 0.617640 0.099196 0.418853 11.00000 0.02381 0.02994 = 0.03055 0.01056 -0.00159 0.00033 AFIX 43 H8 2 0.640096 0.063838 0.447891 11.00000 -1.20000 AFIX 0 C9 1 0.660959 0.142563 0.376358 11.00000 0.02169 0.02827 = 0.02788 0.00664 0.00059 0.00022 AFIX 43 H9 2 0.713477 0.137601 0.376781 11.00000 -1.20000 AFIX 0 C10 1 0.627576 0.193796 0.332687 11.00000 0.02166 0.02213 = 0.02385 0.00350 -0.00066 -0.00178 C11 1 0.550145 0.201115 0.332758 11.00000 0.02199 0.02360 = 0.02922 0.00541 -0.00295 -0.00075 AFIX 43 H11 2 0.527385 0.235546 0.302852 11.00000 -1.20000 AFIX 0 C12 1 0.506299 0.158527 0.376125 11.00000 0.01994 0.02565 = 0.02951 0.00399 -0.00106 -0.00326 AFIX 43 H12 2 0.453834 0.163979 0.376642 11.00000 -1.20000 AFIX 0 C13 1 0.640272 0.252279 0.191847 11.00000 0.02761 0.02710 = 0.02282 0.00196 0.00043 -0.00062 C14 1 0.619949 0.186875 0.161486 11.00000 0.03724 0.02840 = 0.03149 0.00059 -0.00416 -0.00027 AFIX 43 H14 2 0.628545 0.143643 0.186501 11.00000 -1.20000 AFIX 0 C15 1 0.587177 0.185107 0.094720 11.00000 0.03826 0.03907 = 0.03394 -0.00634 -0.00535 -0.00034 AFIX 43 H15 2 0.574136 0.140661 0.073896 11.00000 -1.20000 AFIX 0 C16 1 0.573591 0.248262 0.058649 11.00000 0.04629 0.05061 = 0.02596 0.00026 -0.00504 0.00393 AFIX 43 H16 2 0.551784 0.246954 0.012855 11.00000 -1.20000 AFIX 0 C17 1 0.591695 0.313265 0.089132 11.00000 0.06068 0.03993 = 0.03161 0.00931 -0.01028 0.00247 AFIX 43 H17 2 0.581352 0.356414 0.064581 11.00000 -1.20000 AFIX 0 C18 1 0.625086 0.315556 0.155808 11.00000 0.04970 0.02934 = 0.03095 0.00482 -0.00539 -0.00051 AFIX 43 H18 2 0.637444 0.360201 0.176594 11.00000 -1.20000 AFIX 0 C19 1 0.775346 0.219832 0.278332 11.00000 0.02150 0.02483 = 0.02813 0.00170 0.00427 -0.00133 C20 1 0.792331 0.156952 0.241889 11.00000 0.02764 0.02840 = 0.03702 -0.00491 0.00336 -0.00078 AFIX 43 H20 2 0.756332 0.135264 0.212045 11.00000 -1.20000 AFIX 0 C21 1 0.862278 0.126314 0.249582 11.00000 0.03004 0.03234 = 0.04365 -0.00373 0.00908 0.00224 AFIX 43 H21 2 0.873574 0.082945 0.225805 11.00000 -1.20000 AFIX 0 C22 1 0.915406 0.158564 0.291581 11.00000 0.02475 0.04224 = 0.04612 -0.00103 0.00547 0.00575 AFIX 43 H22 2 0.962671 0.136775 0.297400 11.00000 -1.20000 AFIX 0 C23 1 0.899943 0.222582 0.325228 11.00000 0.02693 0.04935 = 0.05339 -0.01283 -0.00552 0.00364 AFIX 43 H23 2 0.937335 0.245895 0.352170 11.00000 -1.20000 AFIX 0 C24 1 0.829528 0.252681 0.319489 11.00000 0.02814 0.03810 = 0.04177 -0.01169 -0.00407 0.00312 AFIX 43 H24 2 0.818432 0.295814 0.343767 11.00000 -1.20000 AFIX 0 C25 1 0.679467 0.341190 0.315083 11.00000 0.02331 0.02293 = 0.02678 0.00137 0.00018 -0.00076 C26 1 0.725056 0.394113 0.285595 11.00000 0.03269 0.02548 = 0.03627 0.00202 0.00660 -0.00343 AFIX 43 H26 2 0.758286 0.382652 0.248202 11.00000 -1.20000 AFIX 0 C27 1 0.721237 0.463460 0.311510 11.00000 0.04354 0.02436 = 0.04784 0.00235 0.00455 -0.00566 AFIX 43 H27 2 0.751954 0.499624 0.291829 11.00000 -1.20000 AFIX 0 C28 1 0.672603 0.479924 0.366101 11.00000 0.04398 0.02519 = 0.04625 -0.00457 -0.00232 0.00223 AFIX 43 H28 2 0.670070 0.527493 0.383415 11.00000 -1.20000 AFIX 0 C29 1 0.627730 0.427821 0.395622 11.00000 0.03222 0.03315 = 0.03715 -0.00680 0.00165 0.00436 AFIX 43 H29 2 0.594521 0.439717 0.432897 11.00000 -1.20000 AFIX 0 C30 1 0.631303 0.357903 0.370624 11.00000 0.02497 0.02818 = 0.02966 -0.00043 0.00272 -0.00076 AFIX 43 H30 2 0.601157 0.321825 0.391240 11.00000 -1.20000 AFIX 0 HKLF 4 REM JD_POP_OF_0m in Pbca REM wR2 = 0.1854, GooF = S = 1.046, Restrained GooF = 1.127 for all data REM R1 = 0.0579 for 8861 Fo > 4sig(Fo) and 0.0827 for all 12152 data REM 579 parameters refined using 513 restraints END WGHT 0.0962 4.2471 REM Highest difference peak 0.790, deepest hole -0.618, 1-sigma level 0.077 Q1 1 0.7984 0.1154 0.5119 11.00000 0.05 0.51 Q2 1 0.9069 0.0692 0.7116 11.00000 0.05 0.49 Q3 1 0.7637 0.1900 0.5582 11.00000 0.05 0.48 Q4 1 0.8631 0.0835 0.6216 11.00000 0.05 0.43 Q5 1 0.9022 0.1091 0.4809 11.00000 0.05 0.41 Q6 1 0.5816 0.1038 0.4182 11.00000 0.05 0.40 Q7 1 0.6024 0.2770 0.0723 11.00000 0.05 0.39 Q8 1 0.4010 0.0309 0.3314 11.00000 0.05 0.38 Q9 1 0.8197 0.2358 0.3490 11.00000 0.05 0.37 Q10 1 0.6428 0.1660 0.3489 11.00000 0.05 0.37 Q11 1 0.6055 0.1936 0.3331 11.00000 0.05 0.37 Q12 1 0.6422 0.1208 0.3978 11.00000 0.05 0.37 Q13 1 0.2987 0.0438 0.4252 11.00000 0.05 0.36 Q14 1 0.8937 0.2060 0.3615 11.00000 0.05 0.36 Q15 1 0.8821 0.1434 0.2782 11.00000 0.05 0.35 Q16 1 0.8799 0.1756 0.4699 11.00000 0.05 0.35 Q17 1 0.8225 0.1394 0.2537 11.00000 0.05 0.34 Q18 1 0.5198 0.1244 0.3929 11.00000 0.05 0.33 Q19 1 0.5235 0.1823 0.3538 11.00000 0.05 0.33 Q20 1 0.5036 0.0410 0.4341 11.00000 0.05 0.33 Q21 1 0.3426 0.0195 0.4108 11.00000 0.05 0.33 Q22 1 0.6224 0.3110 0.1136 11.00000 0.05 0.32 Q23 1 0.6571 0.3489 0.3440 11.00000 0.05 0.31 Q24 1 0.8441 0.2387 0.5207 11.00000 0.05 0.31 Q25 1 0.9138 0.1903 0.3076 11.00000 0.05 0.31 Q26 1 0.8594 0.1582 0.5595 11.00000 0.05 0.31 Q27 1 0.8990 0.0350 0.5419 11.00000 0.05 0.30 Q28 1 0.6373 0.3882 0.3898 11.00000 0.05 0.30 Q29 1 0.3394 0.1026 0.4991 11.00000 0.05 0.30 Q30 1 0.9045 0.2175 0.6391 11.00000 0.05 0.30 Q31 1 0.7262 0.4289 0.3076 11.00000 0.05 0.30 Q32 1 0.7811 0.2235 0.6054 11.00000 0.05 0.29 Q33 1 0.8170 0.1603 0.6491 11.00000 0.05 0.29 Q34 1 0.3845 0.1686 0.3940 11.00000 0.05 0.29 Q35 1 0.7044 0.3661 0.3010 11.00000 0.05 0.29 Q36 1 0.7986 0.1463 0.6361 11.00000 0.05 0.28 Q37 1 0.8632 0.2395 0.3221 11.00000 0.05 0.28 Q38 1 0.6826 0.2486 0.1615 11.00000 0.05 0.28 Q39 1 0.8592 0.1434 0.6195 11.00000 0.05 0.27 Q40 1 0.7012 0.4717 0.3400 11.00000 0.05 0.27 Q41 1 0.6609 0.3100 0.1499 11.00000 0.05 0.27 Q42 1 0.7841 0.1756 0.2695 11.00000 0.05 0.27 Q43 1 0.9089 -0.0344 0.7100 11.00000 0.05 0.27 Q44 1 0.6798 0.3017 0.3068 11.00000 0.05 0.27 Q45 1 0.8030 0.2345 0.2999 11.00000 0.05 0.27 Q46 1 0.4201 0.1660 0.5153 11.00000 0.05 0.26 Q47 1 0.4040 0.0487 0.4360 11.00000 0.05 0.26 Q48 1 0.6018 0.1855 0.1296 11.00000 0.05 0.26 Q49 1 0.2805 0.0865 0.4729 11.00000 0.05 0.25 Q50 1 1.0032 0.0016 0.7267 11.00000 0.05 0.25 Q51 1 0.7422 0.2394 0.2821 11.00000 0.05 0.25 Q52 1 1.0456 0.0300 0.7404 11.00000 0.05 0.24 Q53 1 0.6570 0.2520 0.2271 11.00000 0.05 0.24 Q54 1 1.0049 0.0717 0.7230 11.00000 0.05 0.24 Q55 1 0.6557 0.2181 0.3204 11.00000 0.05 0.24 Q56 1 0.6594 0.3535 0.3668 11.00000 0.05 0.23 Q57 1 0.9588 0.1181 0.7489 11.00000 0.05 0.23 Q58 1 0.5910 0.2541 0.0485 11.00000 0.05 0.23 Q59 1 0.9584 -0.0338 0.7581 11.00000 0.05 0.23 Q60 1 0.2646 -0.0324 0.3284 11.00000 0.05 0.23 Q61 1 0.6240 0.2806 0.1769 11.00000 0.05 0.22 Q62 1 0.9030 0.0293 0.8904 11.00000 0.05 0.22 Q63 1 1.0255 0.0186 0.7480 11.00000 0.05 0.22 Q64 1 0.9598 0.2502 0.2784 11.00000 0.05 0.22 Q65 1 0.8254 0.1957 0.5524 11.00000 0.05 0.22 Q66 1 0.9384 0.2196 0.5930 11.00000 0.05 0.22 Q67 1 0.7967 0.1969 0.2435 11.00000 0.05 0.22 Q68 1 0.6590 0.4514 0.3887 11.00000 0.05 0.21 Q69 1 0.6594 0.0290 0.4712 11.00000 0.05 0.21 Q70 1 0.4091 0.0774 0.4911 11.00000 0.05 0.21 Q71 1 0.9347 0.2270 0.5478 11.00000 0.05 0.21 Q72 1 0.7028 0.1861 0.0727 11.00000 0.05 0.21 Q73 1 0.7432 0.1168 0.1486 11.00000 0.05 0.21 Q74 1 0.5843 0.3161 -0.0358 11.00000 0.05 0.21 Q75 1 1.0341 -0.0308 0.6695 11.00000 0.05 0.21 Q76 1 0.8421 0.2419 0.5696 11.00000 0.05 0.20 Q77 1 0.9876 0.0099 0.7841 11.00000 0.05 0.20 Q78 1 0.8593 0.1339 0.5178 11.00000 0.05 0.20 Q79 1 0.6427 0.5292 0.3553 11.00000 0.05 0.20 Q80 1 0.9422 -0.0423 0.6221 11.00000 0.05 0.20 Q81 1 0.7389 0.4639 0.3170 11.00000 0.05 0.20 Q82 1 1.0600 -0.0201 0.6286 11.00000 0.05 0.20 Q83 1 0.9605 0.1397 0.5610 11.00000 0.05 0.20 Q84 1 0.5425 0.3895 0.4149 11.00000 0.05 0.20 Q85 1 0.9548 0.1992 0.5597 11.00000 0.05 0.19 Q86 1 0.8957 0.1738 0.3316 11.00000 0.05 0.19 Q87 1 0.6645 0.1509 0.0620 11.00000 0.05 0.19 Q88 1 0.4169 0.2130 0.5323 11.00000 0.05 0.19 Q89 1 0.5262 0.1289 0.1287 11.00000 0.05 0.19 Q90 1 0.8651 0.2314 0.5903 11.00000 0.05 0.19 Q91 1 1.0029 -0.0148 0.6160 11.00000 0.05 0.19 Q92 1 0.2955 0.1340 0.5086 11.00000 0.05 0.19 Q93 1 1.0009 -0.0619 0.6062 11.00000 0.05 0.19 Q94 1 0.2619 0.1550 0.4681 11.00000 0.05 0.19 Q95 1 0.5035 0.4360 0.4683 11.00000 0.05 0.19 Q96 1 0.6379 0.3066 0.0775 11.00000 0.05 0.19 Q97 1 0.9371 0.0762 0.4507 11.00000 0.05 0.18 Q98 1 0.8865 0.3351 0.3436 11.00000 0.05 0.18 Q99 1 1.0163 0.0869 0.7484 11.00000 0.05 0.18 Q100 1 0.9594 0.1637 0.6132 11.00000 0.05 0.17 Q101 1 0.6805 0.2580 0.3875 11.00000 0.05 0.17 Q102 1 0.2966 0.1466 0.4219 11.00000 0.05 0.17 Q103 1 0.8160 0.2998 0.3918 11.00000 0.05 0.17 Q104 1 0.9999 0.1438 0.2701 11.00000 0.05 0.17 Q105 1 0.8823 0.0805 0.2530 11.00000 0.05 0.17 Q106 1 0.3388 -0.0749 0.3890 11.00000 0.05 0.17 Q107 1 0.6721 0.2527 0.0519 11.00000 0.05 0.17 Q108 1 0.8206 0.0207 0.5879 11.00000 0.05 0.17 Q109 1 0.5987 0.2196 -0.0326 11.00000 0.05 0.17 Q110 1 0.5415 0.3855 0.1288 11.00000 0.05 0.17 Q111 1 0.9226 0.2183 0.2090 11.00000 0.05 0.17 Q112 1 0.5376 0.1151 0.1378 11.00000 0.05 0.17 Q113 1 0.5787 0.5741 0.4018 11.00000 0.05 0.17 Q114 1 0.6796 0.5236 0.4093 11.00000 0.05 0.17 Q115 1 0.1996 0.1669 0.4730 11.00000 0.05 0.17 Q116 1 0.3746 0.1130 0.4715 11.00000 0.05 0.17 Q117 1 1.0206 -0.0501 0.6166 11.00000 0.05 0.17 Q118 1 0.7053 0.5536 0.4103 11.00000 0.05 0.17 Q119 1 0.5160 0.1539 0.0679 11.00000 0.05 0.17 Q120 1 0.4804 0.2861 0.0411 11.00000 0.05 0.17 ; _shelx_res_checksum 36580 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F2 F 0.91052(11) 0.06642(13) 0.80056(10) 0.0579(5) Uani 0.8456(13) 1 d D U P A 1 F3 F 0.99003(15) -0.01042(14) 0.76345(14) 0.0896(8) Uani 0.8456(13) 1 d D U P A 1 F4 F 1.00043(11) 0.10207(14) 0.73473(11) 0.0690(6) Uani 0.8456(13) 1 d D U P A 1 C31 C 0.95299(17) 0.04887(19) 0.74575(17) 0.0465(6) Uani 0.8456(13) 1 d D U P A 1 S1 S 0.89722(6) 0.03031(8) 0.66674(7) 0.03589(19) Uani 0.8456(13) 1 d D U P A 1 O2 O 0.84202(13) -0.01939(11) 0.69262(13) 0.0506(5) Uani 0.8456(13) 1 d D U P A 1 O3 O 0.94914(13) 0.00661(13) 0.61476(12) 0.0562(5) Uani 0.8456(13) 1 d D U P A 1 N1 N 0.85724(11) 0.10402(10) 0.65296(11) 0.0369(4) Uani 0.8456(13) 1 d D U P A 1 F5 F 0.76099(13) 0.15235(19) 0.53720(15) 0.1074(10) Uani 0.8456(13) 1 d D U P A 1 F6 F 0.8473(2) 0.0927(2) 0.49469(16) 0.1225(12) Uani 0.8456(13) 1 d D U P A 1 F7 F 0.84638(19) 0.20745(18) 0.48028(13) 0.1036(10) Uani 0.8456(13) 1 d D U P A 1 C32 C 0.8333(2) 0.1536(2) 0.52463(17) 0.0672(8) Uani 0.8456(13) 1 d D U P A 1 S2 S 0.88667(3) 0.16628(3) 0.60472(3) 0.03088(13) Uani 0.8456(13) 1 d D U P A 1 O4 O 0.86055(17) 0.23338(13) 0.63094(15) 0.0614(7) Uani 0.8456(13) 1 d D U P A 1 O5 O 0.96209(10) 0.16255(12) 0.58270(13) 0.0536(5) Uani 0.8456(13) 1 d D U P A 1 F2B F 0.9151(7) 0.1041(7) 0.7812(6) 0.066(2) Uani 0.1544(13) 1 d D U P A 2 F3B F 0.9456(8) -0.0066(7) 0.7932(7) 0.079(2) Uani 0.1544(13) 1 d D U P A 2 F4B F 1.0261(6) 0.0597(8) 0.7483(7) 0.072(2) Uani 0.1544(13) 1 d D U P A 2 C31B C 0.9535(9) 0.0507(10) 0.7530(8) 0.060(2) Uani 0.1544(13) 1 d D U P A 2 S1B S 0.9166(4) 0.0283(5) 0.6651(5) 0.0472(14) Uani 0.1544(13) 1 d D U P A 2 O2B O 0.8416(6) 0.0110(7) 0.6793(7) 0.049(2) Uani 0.1544(13) 1 d D U P A 2 O3B O 0.9662(7) -0.0252(6) 0.6391(7) 0.058(2) Uani 0.1544(13) 1 d D U P A 2 N1B N 0.9332(7) 0.1054(6) 0.6327(6) 0.0470(17) Uani 0.1544(13) 1 d D U P A 2 F5B F 0.7734(7) 0.1440(8) 0.5992(7) 0.085(2) Uani 0.1544(13) 1 d D U P A 2 F6B F 0.8271(8) 0.2278(8) 0.6130(8) 0.075(2) Uani 0.1544(13) 1 d D U P A 2 F7B F 0.8030(9) 0.2038(9) 0.5028(7) 0.093(2) Uani 0.1544(13) 1 d D U P A 2 C32B C 0.8259(8) 0.1798(8) 0.5643(8) 0.0724(19) Uani 0.1544(13) 1 d D U P A 2 S2B S 0.9060(2) 0.1250(2) 0.55971(19) 0.0481(8) Uani 0.1544(13) 1 d D U P A 2 O4B O 0.8897(10) 0.0762(9) 0.5060(8) 0.072(3) Uani 0.1544(13) 1 d D U P A 2 O5B O 0.9627(7) 0.1720(8) 0.5278(8) 0.067(2) Uani 0.1544(13) 1 d D U P A 2 P1 P 0.68160(2) 0.25254(2) 0.27873(2) 0.02198(9) Uani 1 1 d . . . . . F1 F 0.41903(13) 0.14668(14) 0.54826(14) 0.0693(8) Uani 0.683(4) 1 d . . P B 1 F1B F 0.4293(2) -0.0132(2) 0.3728(2) 0.0496(13) Uani 0.317(4) 1 d . . P B 2 O1 O 0.50213(7) 0.06433(8) 0.46417(8) 0.0395(3) Uani 1 1 d . . . . . C1 C 0.42513(9) 0.06351(10) 0.46015(10) 0.0349(4) Uani 1 1 d . . . . . C2 C 0.38343(12) 0.10403(13) 0.50557(14) 0.0476(5) Uani 1 1 d . . . . . H2 H 0.407767 0.134820 0.538133 0.057 Uiso 0.317(4) 1 calc R U P B 2 C3 C 0.30688(13) 0.10112(16) 0.50506(15) 0.0566(6) Uani 1 1 d . . . . . H3 H 0.278937 0.129449 0.537189 0.068 Uiso 1 1 calc R U . . . C4 C 0.27117(11) 0.05692(13) 0.45772(13) 0.0465(5) Uani 1 1 d . . . . . H4 H 0.218432 0.055249 0.456653 0.056 Uiso 1 1 calc R U . . . C5 C 0.31198(11) 0.01506(12) 0.41186(11) 0.0413(4) Uani 1 1 d . . . . . H5 H 0.287665 -0.015876 0.379416 0.050 Uiso 1 1 calc R U . . . C6 C 0.38910(10) 0.01868(11) 0.41367(11) 0.0381(4) Uani 1 1 d . . . . . H6 H 0.417379 -0.010238 0.382343 0.046 Uiso 0.683(4) 1 calc R U P B 1 C7 C 0.54058(8) 0.10783(8) 0.41872(8) 0.0255(3) Uani 1 1 d . . . . . C8 C 0.61764(8) 0.09920(9) 0.41885(9) 0.0281(3) Uani 1 1 d . . . . . H8 H 0.640096 0.063838 0.447891 0.034 Uiso 1 1 calc R U . . . C9 C 0.66096(8) 0.14256(8) 0.37636(8) 0.0259(3) Uani 1 1 d . . . . . H9 H 0.713477 0.137601 0.376781 0.031 Uiso 1 1 calc R U . . . C10 C 0.62758(8) 0.19380(8) 0.33269(8) 0.0225(2) Uani 1 1 d . . . . . C11 C 0.55014(8) 0.20112(8) 0.33276(8) 0.0249(3) Uani 1 1 d . . . . . H11 H 0.527385 0.235546 0.302852 0.030 Uiso 1 1 calc R U . . . C12 C 0.50630(8) 0.15853(8) 0.37612(8) 0.0250(3) Uani 1 1 d . . . . . H12 H 0.453834 0.163979 0.376642 0.030 Uiso 1 1 calc R U . . . C13 C 0.64027(9) 0.25228(8) 0.19185(8) 0.0258(3) Uani 1 1 d . . . . . C14 C 0.61995(10) 0.18687(9) 0.16149(9) 0.0324(3) Uani 1 1 d . . . . . H14 H 0.628545 0.143643 0.186501 0.039 Uiso 1 1 calc R U . . . C15 C 0.58718(11) 0.18511(11) 0.09472(10) 0.0371(4) Uani 1 1 d . . . . . H15 H 0.574136 0.140661 0.073896 0.045 Uiso 1 1 calc R U . . . C16 C 0.57359(12) 0.24826(12) 0.05865(10) 0.0410(4) Uani 1 1 d . . . . . H16 H 0.551784 0.246954 0.012855 0.049 Uiso 1 1 calc R U . . . C17 C 0.59169(13) 0.31326(12) 0.08913(11) 0.0441(5) Uani 1 1 d . . . . . H17 H 0.581352 0.356414 0.064581 0.053 Uiso 1 1 calc R U . . . C18 C 0.62509(12) 0.31556(10) 0.15581(10) 0.0367(4) Uani 1 1 d . . . . . H18 H 0.637444 0.360201 0.176594 0.044 Uiso 1 1 calc R U . . . C19 C 0.77535(8) 0.21983(8) 0.27833(8) 0.0248(3) Uani 1 1 d . . . . . C20 C 0.79233(9) 0.15695(9) 0.24189(10) 0.0310(3) Uani 1 1 d . . . . . H20 H 0.756332 0.135264 0.212045 0.037 Uiso 1 1 calc R U . . . C21 C 0.86228(10) 0.12631(10) 0.24958(11) 0.0353(4) Uani 1 1 d . . . . . H21 H 0.873574 0.082945 0.225805 0.042 Uiso 1 1 calc R U . . . C22 C 0.91541(10) 0.15856(11) 0.29158(11) 0.0377(4) Uani 1 1 d . . . . . H22 H 0.962671 0.136775 0.297400 0.045 Uiso 1 1 calc R U . . . C23 C 0.89994(10) 0.22258(12) 0.32523(13) 0.0432(5) Uani 1 1 d . . . . . H23 H 0.937335 0.245895 0.352170 0.052 Uiso 1 1 calc R U . . . C24 C 0.82953(10) 0.25268(10) 0.31949(11) 0.0360(4) Uani 1 1 d . . . . . H24 H 0.818432 0.295814 0.343767 0.043 Uiso 1 1 calc R U . . . C25 C 0.67947(8) 0.34119(8) 0.31508(8) 0.0243(3) Uani 1 1 d . . . . . C26 C 0.72506(10) 0.39411(9) 0.28559(10) 0.0315(3) Uani 1 1 d . . . . . H26 H 0.758286 0.382652 0.248202 0.038 Uiso 1 1 calc R U . . . C27 C 0.72124(12) 0.46346(9) 0.31151(11) 0.0386(4) Uani 1 1 d . . . . . H27 H 0.751954 0.499624 0.291829 0.046 Uiso 1 1 calc R U . . . C28 C 0.67260(11) 0.47992(10) 0.36610(11) 0.0385(4) Uani 1 1 d . . . . . H28 H 0.670070 0.527493 0.383415 0.046 Uiso 1 1 calc R U . . . C29 C 0.62773(10) 0.42782(10) 0.39562(10) 0.0342(3) Uani 1 1 d . . . . . H29 H 0.594521 0.439717 0.432897 0.041 Uiso 1 1 calc R U . . . C30 C 0.63130(9) 0.35790(9) 0.37062(9) 0.0276(3) Uani 1 1 d . . . . . H30 H 0.601157 0.321825 0.391240 0.033 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F2 0.0558(10) 0.0784(13) 0.0395(9) 0.0017(9) 0.0022(7) 0.0011(10) F3 0.0829(15) 0.1019(17) 0.0839(15) 0.0210(13) -0.0150(12) 0.0518(13) F4 0.0450(9) 0.1024(16) 0.0598(11) 0.0010(11) -0.0083(8) -0.0251(10) C31 0.0343(11) 0.0595(14) 0.0457(13) 0.0118(12) -0.0018(10) 0.0082(10) S1 0.0354(4) 0.0308(3) 0.0414(3) -0.0022(2) 0.0045(3) 0.0011(3) O2 0.0531(11) 0.0307(9) 0.0681(14) 0.0036(9) 0.0084(9) -0.0082(8) O3 0.0581(12) 0.0511(12) 0.0593(13) -0.0120(10) 0.0186(10) 0.0090(10) N1 0.0318(8) 0.0382(9) 0.0407(9) 0.0089(7) 0.0048(7) 0.0009(7) F5 0.0610(13) 0.160(2) 0.1012(18) 0.0515(17) -0.0424(12) -0.0339(14) F6 0.183(3) 0.120(2) 0.0652(15) -0.0432(16) -0.028(2) -0.034(2) F7 0.113(2) 0.138(2) 0.0596(13) 0.0541(14) -0.0190(14) -0.0312(19) C32 0.0746(18) 0.086(2) 0.0405(13) 0.0124(14) -0.0176(13) -0.0270(16) S2 0.0322(2) 0.0310(2) 0.0294(2) -0.00145(17) -0.00076(17) -0.00439(17) O4 0.0848(18) 0.0359(9) 0.0633(15) -0.0085(10) 0.0200(13) -0.0035(11) O5 0.0323(8) 0.0600(11) 0.0685(13) 0.0180(10) 0.0066(8) -0.0076(8) F2B 0.065(4) 0.082(4) 0.049(4) -0.006(4) 0.000(4) 0.006(4) F3B 0.076(4) 0.088(4) 0.074(4) 0.024(4) -0.009(4) 0.009(4) F4B 0.050(4) 0.096(5) 0.069(4) 0.016(4) -0.006(4) -0.009(4) C31B 0.052(3) 0.073(3) 0.056(3) 0.009(3) -0.005(3) 0.004(3) S1B 0.047(3) 0.0319(18) 0.063(2) 0.0095(16) 0.003(2) 0.000(2) O2B 0.043(4) 0.046(4) 0.059(4) 0.004(4) 0.005(3) -0.012(4) O3B 0.062(5) 0.043(4) 0.070(5) 0.002(4) 0.017(4) 0.010(4) N1B 0.044(3) 0.044(3) 0.052(3) 0.007(3) -0.003(3) -0.004(3) F5B 0.074(4) 0.099(4) 0.080(4) 0.013(4) 0.000(4) -0.012(4) F6B 0.084(5) 0.066(4) 0.074(5) -0.009(4) 0.001(4) 0.000(4) F7B 0.088(5) 0.122(5) 0.069(4) 0.034(4) -0.030(4) -0.015(5) C32B 0.072(3) 0.086(3) 0.059(3) 0.013(3) -0.010(3) -0.017(3) S2B 0.0533(17) 0.0510(18) 0.0401(16) -0.0026(13) -0.0044(13) -0.0063(14) O4B 0.088(5) 0.083(5) 0.046(4) -0.038(4) -0.017(4) 0.004(5) O5B 0.060(5) 0.076(5) 0.067(5) 0.009(4) 0.004(4) -0.008(4) P1 0.02169(16) 0.02103(16) 0.02321(17) 0.00263(12) 0.00141(12) -0.00138(12) F1 0.0528(13) 0.0776(17) 0.0775(16) -0.0402(13) -0.0065(11) -0.0178(11) F1B 0.049(2) 0.051(2) 0.048(2) -0.0142(18) 0.0076(17) 0.0036(18) O1 0.0245(5) 0.0472(7) 0.0467(7) 0.0260(6) -0.0006(5) -0.0073(5) C1 0.0250(7) 0.0380(9) 0.0417(9) 0.0152(7) 0.0020(6) -0.0063(6) C2 0.0349(9) 0.0517(12) 0.0561(13) -0.0066(10) 0.0023(9) -0.0118(8) C3 0.0358(10) 0.0666(15) 0.0673(16) -0.0181(13) 0.0126(10) -0.0057(10) C4 0.0262(8) 0.0585(13) 0.0548(12) 0.0020(10) 0.0035(8) -0.0086(8) C5 0.0344(9) 0.0486(11) 0.0410(10) 0.0053(8) -0.0025(7) -0.0111(8) C6 0.0324(8) 0.0446(10) 0.0374(9) 0.0096(8) 0.0034(7) -0.0025(7) C7 0.0229(6) 0.0274(7) 0.0264(7) 0.0058(5) -0.0011(5) -0.0052(5) C8 0.0238(6) 0.0299(7) 0.0305(7) 0.0106(6) -0.0016(5) 0.0003(5) C9 0.0217(6) 0.0283(7) 0.0279(7) 0.0066(5) 0.0006(5) 0.0002(5) C10 0.0217(6) 0.0221(6) 0.0239(6) 0.0035(5) -0.0007(5) -0.0018(5) C11 0.0220(6) 0.0236(6) 0.0292(7) 0.0054(5) -0.0030(5) -0.0007(5) C12 0.0199(6) 0.0256(6) 0.0295(7) 0.0040(5) -0.0011(5) -0.0033(5) C13 0.0276(6) 0.0271(7) 0.0228(6) 0.0020(5) 0.0004(5) -0.0006(5) C14 0.0372(8) 0.0284(7) 0.0315(8) 0.0006(6) -0.0042(6) -0.0003(6) C15 0.0383(9) 0.0391(9) 0.0339(8) -0.0063(7) -0.0053(7) -0.0003(7) C16 0.0463(10) 0.0506(11) 0.0260(8) 0.0003(7) -0.0050(7) 0.0039(8) C17 0.0607(13) 0.0399(10) 0.0316(9) 0.0093(7) -0.0103(8) 0.0025(9) C18 0.0497(10) 0.0293(8) 0.0310(8) 0.0048(6) -0.0054(7) -0.0005(7) C19 0.0215(6) 0.0248(6) 0.0281(7) 0.0017(5) 0.0043(5) -0.0013(5) C20 0.0276(7) 0.0284(7) 0.0370(8) -0.0049(6) 0.0034(6) -0.0008(5) C21 0.0300(7) 0.0323(8) 0.0437(9) -0.0037(7) 0.0091(7) 0.0022(6) C22 0.0247(7) 0.0422(9) 0.0461(10) -0.0010(8) 0.0055(7) 0.0057(6) C23 0.0269(8) 0.0494(11) 0.0534(12) -0.0128(9) -0.0055(7) 0.0036(7) C24 0.0281(7) 0.0381(9) 0.0418(9) -0.0117(7) -0.0041(7) 0.0031(6) C25 0.0233(6) 0.0229(6) 0.0268(6) 0.0014(5) 0.0002(5) -0.0008(5) C26 0.0327(7) 0.0255(7) 0.0363(8) 0.0020(6) 0.0066(6) -0.0034(6) C27 0.0435(9) 0.0244(7) 0.0478(10) 0.0023(7) 0.0046(8) -0.0057(7) C28 0.0440(10) 0.0252(7) 0.0462(10) -0.0046(7) -0.0023(8) 0.0022(7) C29 0.0322(8) 0.0332(8) 0.0371(9) -0.0068(7) 0.0016(6) 0.0044(6) C30 0.0250(6) 0.0282(7) 0.0297(7) -0.0004(6) 0.0027(5) -0.0008(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F2 C31 F4 107.8(3) . . ? F2 C31 F3 107.3(3) . . ? F4 C31 F3 109.9(3) . . ? F2 C31 S1 111.5(2) . . ? F4 C31 S1 111.5(2) . . ? F3 C31 S1 108.6(2) . . ? O3 S1 O2 118.84(16) . . ? O3 S1 N1 117.23(16) . . ? O2 S1 N1 107.77(13) . . ? O3 S1 C31 105.10(15) . . ? O2 S1 C31 102.91(17) . . ? N1 S1 C31 102.61(15) . . ? S2 N1 S1 126.20(13) . . ? F6 C32 F5 104.7(3) . . ? F6 C32 F7 110.9(3) . . ? F5 C32 F7 107.5(4) . . ? F6 C32 S2 112.1(3) . . ? F5 C32 S2 112.0(3) . . ? F7 C32 S2 109.4(2) . . ? O5 S2 O4 117.29(15) . . ? O5 S2 N1 117.06(11) . . ? O4 S2 N1 109.89(13) . . ? O5 S2 C32 104.88(17) . . ? O4 S2 C32 103.30(19) . . ? N1 S2 C32 102.03(14) . . ? F4B C31B F3B 104.4(14) . . ? F4B C31B F2B 116.5(15) . . ? F3B C31B F2B 109.0(15) . . ? F4B C31B S1B 109.0(11) . . ? F3B C31B S1B 107.2(12) . . ? F2B C31B S1B 110.3(11) . . ? O2B S1B O3B 120.0(9) . . ? O2B S1B N1B 117.3(8) . . ? O3B S1B N1B 112.7(8) . . ? O2B S1B C31B 103.1(9) . . ? O3B S1B C31B 104.2(9) . . ? N1B S1B C31B 94.2(8) . . ? S2B N1B S1B 120.7(8) . . ? F6B C32B F7B 113.5(15) . . ? F6B C32B F5B 90.5(13) . . ? F7B C32B F5B 112.8(14) . . ? F6B C32B S2B 115.2(12) . . ? F7B C32B S2B 114.3(12) . . ? F5B C32B S2B 108.1(11) . . ? O4B S2B O5B 103.9(10) . . ? O4B S2B N1B 125.0(9) . . ? O5B S2B N1B 107.0(7) . . ? O4B S2B C32B 104.0(9) . . ? O5B S2B C32B 103.7(8) . . ? N1B S2B C32B 111.2(7) . . ? C10 P1 C19 107.69(7) . . ? C10 P1 C25 109.83(7) . . ? C19 P1 C25 109.68(7) . . ? C10 P1 C13 107.03(7) . . ? C19 P1 C13 112.54(7) . . ? C25 P1 C13 109.97(7) . . ? C7 O1 C1 118.45(13) . . ? C2 C1 C6 118.61(17) . . ? C2 C1 O1 120.46(19) . . ? C6 C1 O1 120.80(18) . . ? F1 C2 C1 117.2(2) . . ? F1 C2 C3 121.3(2) . . ? C1 C2 C3 121.4(2) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.00(19) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 119.2(2) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? F1B C6 C1 115.1(3) . . ? F1B C6 C5 123.7(3) . . ? C1 C6 C5 121.1(2) . . ? C1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? O1 C7 C12 122.98(13) . . ? O1 C7 C8 115.57(13) . . ? C12 C7 C8 121.43(13) . . ? C9 C8 C7 119.42(14) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 120.14(14) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.57(13) . . ? C11 C10 P1 118.81(11) . . ? C9 C10 P1 121.59(11) . . ? C12 C11 C10 120.65(13) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C7 C12 C11 118.78(13) . . ? C7 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C18 C13 C14 119.49(16) . . ? C18 C13 P1 121.57(13) . . ? C14 C13 P1 118.88(12) . . ? C15 C14 C13 120.13(17) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.95(18) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.25(18) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.21(18) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.92(18) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C24 C19 C20 119.63(15) . . ? C24 C19 P1 120.40(12) . . ? C20 C19 P1 119.68(12) . . ? C21 C20 C19 119.60(16) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.41(17) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.17(17) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.86(18) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.22(17) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C30 C25 C26 120.22(14) . . ? C30 C25 P1 120.48(11) . . ? C26 C25 P1 119.27(12) . . ? C27 C26 C25 119.46(16) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C28 C27 C26 120.05(17) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C29 C28 C27 120.73(16) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 119.94(17) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 119.59(15) . . ? C29 C30 H30 120.2 . . ? C25 C30 H30 120.2 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F2 C31 1.328(4) . ? F3 C31 1.338(4) . ? F4 C31 1.329(4) . ? C31 S1 1.831(3) . ? S1 O3 1.426(2) . ? S1 O2 1.446(2) . ? S1 N1 1.578(2) . ? N1 S2 1.5716(19) . ? F5 C32 1.323(4) . ? F6 C32 1.298(5) . ? F7 C32 1.332(4) . ? C32 S2 1.808(3) . ? S2 O5 1.4216(19) . ? S2 O4 1.430(2) . ? F2B C31B 1.326(16) . ? F3B C31B 1.322(16) . ? F4B C31B 1.321(16) . ? C31B S1B 1.836(14) . ? S1B O2B 1.415(11) . ? S1B O3B 1.428(11) . ? S1B N1B 1.595(12) . ? N1B S2B 1.508(10) . ? F5B C32B 1.334(15) . ? F6B C32B 1.288(16) . ? F7B C32B 1.312(15) . ? C32B S2B 1.772(13) . ? S2B O4B 1.396(11) . ? S2B O5B 1.477(11) . ? P1 C10 1.7871(14) . ? P1 C19 1.7954(15) . ? P1 C25 1.7969(16) . ? P1 C13 1.8015(16) . ? F1 C2 1.303(3) . ? F1B C6 1.215(4) . ? O1 C7 1.3709(18) . ? O1 C1 1.388(2) . ? C1 C2 1.369(3) . ? C1 C6 1.377(3) . ? C2 C3 1.379(3) . ? C2 H2 0.9500 . ? C3 C4 1.378(3) . ? C3 H3 0.9500 . ? C4 C5 1.380(3) . ? C4 H4 0.9500 . ? C5 C6 1.390(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.389(2) . ? C7 C8 1.397(2) . ? C8 C9 1.383(2) . ? C8 H8 0.9500 . ? C9 C10 1.401(2) . ? C9 H9 0.9500 . ? C10 C11 1.401(2) . ? C11 C12 1.389(2) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.394(2) . ? C13 C14 1.401(2) . ? C14 C15 1.392(3) . ? C14 H14 0.9500 . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 C17 1.385(3) . ? C16 H16 0.9500 . ? C17 C18 1.396(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.391(2) . ? C19 C20 1.398(2) . ? C20 C21 1.391(2) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.391(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.396(2) . ? C25 C26 1.402(2) . ? C26 C27 1.389(2) . ? C26 H26 0.9500 . ? C27 C28 1.387(3) . ? C27 H27 0.9500 . ? C28 C29 1.384(3) . ? C28 H28 0.9500 . ? C29 C30 1.393(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ?