#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:52:58 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253999 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240484.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_7240484 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_absolute_configuration ad _chemical_formula_moiety 'C30 H24 O P, C2 F6 N O4 S2' _chemical_formula_sum 'C32 H24 F6 N O5 P S2' _chemical_formula_weight 711.61 _chemical_name_systematic '(4-phenoxyphenyl)triphenylphosphonium bistriflimide' _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _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 4 _cell_length_a 18.1884(8) _cell_length_b 9.1975(4) _cell_length_c 18.6788(7) _cell_measurement_reflns_used 9332 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 80.5363 _cell_measurement_theta_min 5.3895 _cell_volume 3124.7(2) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2016)' _computing_data_collection 'Apex3 v2018.7-2 (Bruker, 2017)' _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 7.4074 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type ; Bruker AXS D8 Quest CMOS diffractometer with PhotonII charge-integrating pixel array detector (CPAD) ; _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator 'laterally graded multilayer (Goebel) mirror' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 34993 _diffrn_reflns_point_group_measured_fraction_full 0.840 _diffrn_reflns_point_group_measured_fraction_max 0.806 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 80.721 _diffrn_reflns_theta_min 4.863 _diffrn_source 'I-mu-S microsource X-ray tube' _diffrn_source_current '1.0 mA' _diffrn_source_voltage '50 kV' _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_T_max 0.7543 _exptl_absorpt_correction_T_min 0.5348 _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 1.513 _exptl_crystal_description plate _exptl_crystal_F_000 1456 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.070 _refine_diff_density_max 0.205 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.038(19) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 561 _refine_ls_number_reflns 5537 _refine_ls_number_restraints 532 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0303 _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^)+(0.0371P)^2^+0.8875P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.0813 _reflns_Friedel_coverage 0.581 _reflns_Friedel_fraction_full 0.672 _reflns_Friedel_fraction_max 0.612 _reflns_number_gt 5354 _reflns_number_total 5537 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cp01214a2.cif _cod_data_source_block JD_POP_0m _cod_depositor_comments 'Adding full bibliography for 7240483--7240486.cif.' _cod_database_code 7240484 _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 0.597 _shelx_estimated_absorpt_t_max 0.831 _shelx_res_file ; TITL JD_POP_0m in Pca2(1) JD_POP_0m.res created by SHELXL-2018/3 at 11:53:17 on 25-May-2019 CELL 1.54178 18.1884 9.1975 18.6788 90.0000 90.0000 90.0000 ZERR 4.00 0.0008 0.0004 0.0007 0.0000 0.0000 0.0000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5+X, -Y, Z SYMM 0.5-X, Y, 0.5+Z SFAC C H N O F P S UNIT 128 96 4 20 24 4 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.170 SIZE 0.21 0.14 0.07 L.S. 4 BOND $H ACTA CONF FMAP 2 PLAN 20 SIMU 0.01 F1 > F6B TWIN WGHT 0.037100 0.887500 BASF 0.03831 FVAR 0.62655 0.78316 PART 1 21 F1 5 0.584588 0.376656 0.622536 21.00000 0.06301 0.04307 = 0.08347 -0.00731 -0.00238 0.00392 F2 5 0.496014 0.433104 0.691821 21.00000 0.07708 0.07180 = 0.07707 0.01694 0.03037 -0.01867 F3 5 0.497941 0.511891 0.583620 21.00000 0.06963 0.05323 = 0.06815 0.00741 -0.02783 -0.01245 S1 7 0.589163 0.642342 0.672321 21.00000 0.04748 0.04034 = 0.02620 0.00206 0.00381 0.00149 C31 1 0.539026 0.481842 0.639591 21.00000 0.04702 0.04239 = 0.04384 0.00946 0.00328 -0.00050 O2 4 0.534123 0.740455 0.696621 21.00000 0.05925 0.04874 = 0.04499 -0.00259 0.01202 0.01304 O3 4 0.639315 0.583021 0.724133 21.00000 0.06377 0.05545 = 0.03323 0.00590 -0.00662 0.00343 N1 3 0.636664 0.690373 0.605400 21.00000 0.03954 0.04228 = 0.03716 0.00320 -0.00032 -0.00100 O4 4 0.531726 0.818366 0.540274 21.00000 0.04322 0.06357 = 0.05552 0.01980 -0.01107 -0.00621 O5 4 0.647866 0.762241 0.480787 21.00000 0.08184 0.07327 = 0.03483 0.00451 0.00781 -0.00125 S2 7 0.608774 0.796234 0.544790 21.00000 0.04346 0.04341 = 0.02615 0.00213 -0.00317 -0.00799 C32 1 0.644188 0.973050 0.572718 21.00000 0.07598 0.05142 = 0.04867 0.01494 -0.01319 -0.01506 F4 5 0.622280 1.008470 0.635627 21.00000 0.17258 0.05365 = 0.05745 -0.01488 0.00546 -0.01938 F5 5 0.621927 1.072379 0.525683 21.00000 0.12951 0.05137 = 0.08629 0.03297 -0.03406 -0.02457 F6 5 0.716980 0.973785 0.571597 21.00000 0.08035 0.10174 = 0.10693 0.01590 -0.03192 -0.04620 PART 2 -21 SAME F1 > F6 F1B 5 0.555914 0.387177 0.683101 -21.00000 0.07885 0.06235 = 0.08230 0.04283 -0.00956 -0.00166 F2B 5 0.467913 0.487689 0.630424 -21.00000 0.03883 0.06390 = 0.08380 0.02002 -0.00912 -0.01004 F3B 5 0.571031 0.458645 0.575865 -21.00000 0.08742 0.05667 = 0.06308 -0.00728 0.01113 -0.01091 S1B 7 0.573678 0.668451 0.671838 -21.00000 0.05272 0.05006 = 0.02715 0.00604 -0.00057 -0.00681 C31B 1 0.540668 0.491753 0.637673 -21.00000 0.05275 0.05006 = 0.04620 0.01062 0.00187 0.00214 O2B 4 0.526770 0.695322 0.731528 -21.00000 0.08113 0.07412 = 0.03956 0.00776 0.01247 -0.01493 O3B 4 0.649815 0.642341 0.683078 -21.00000 0.02720 0.06898 = 0.06068 0.01918 -0.01434 -0.00706 N1B 3 0.553088 0.775002 0.607733 -21.00000 0.04425 0.04729 = 0.03837 0.00359 -0.00184 -0.00488 O4B 4 0.562989 0.861942 0.486541 -21.00000 0.08643 0.07960 = 0.03823 0.01277 -0.01840 -0.02844 O5B 4 0.668509 0.731415 0.534189 -21.00000 0.07352 0.05494 = 0.06021 0.01026 0.03295 0.00942 S2B 7 0.606355 0.817572 0.545277 -21.00000 0.06057 0.04976 = 0.03051 0.01799 -0.00270 -0.00972 C32B 1 0.644586 0.991674 0.573997 -21.00000 0.07818 0.04611 = 0.04985 0.00942 -0.01446 -0.01880 F4B 5 0.693209 1.040211 0.529726 -21.00000 0.09529 0.05876 = 0.08630 0.03452 -0.00635 -0.03046 F5B 5 0.592311 1.091078 0.582340 -21.00000 0.13536 0.05687 = 0.08569 0.00041 -0.00775 0.02682 F6B 5 0.675973 0.982069 0.637038 -21.00000 0.10541 0.07358 = 0.07570 -0.00538 -0.03045 -0.02866 PART 0 P1 6 0.318034 0.554644 0.449992 11.00000 0.03030 0.02788 = 0.02247 -0.00138 0.00011 0.00079 O1 4 0.511147 0.914781 0.265745 11.00000 0.04283 0.04641 = 0.04785 0.01914 0.01068 0.00369 C1 1 0.376282 0.660478 0.393046 11.00000 0.03162 0.02787 = 0.02481 -0.00235 0.00136 0.00163 C2 1 0.452756 0.652255 0.402011 11.00000 0.03384 0.03140 = 0.02911 0.00209 0.00038 0.00328 AFIX 43 H2 2 0.472694 0.588693 0.437086 11.00000 -1.20000 AFIX 0 C3 1 0.499420 0.735482 0.360447 11.00000 0.03162 0.03230 = 0.03223 0.00039 0.00460 0.00048 AFIX 43 H3 2 0.551138 0.729938 0.367011 11.00000 -1.20000 AFIX 0 C4 1 0.469705 0.827673 0.308771 11.00000 0.04052 0.02878 = 0.02845 0.00101 0.00895 0.00071 C5 1 0.394169 0.836154 0.299228 11.00000 0.04105 0.03466 = 0.02970 0.00486 0.00023 0.00537 AFIX 43 H5 2 0.374426 0.898853 0.263675 11.00000 -1.20000 AFIX 0 C6 1 0.347550 0.753722 0.341255 11.00000 0.03362 0.03331 = 0.02814 -0.00057 -0.00062 0.00439 AFIX 43 H6 2 0.295851 0.760596 0.334850 11.00000 -1.20000 AFIX 0 C7 1 0.587995 0.904835 0.270159 11.00000 0.04521 0.03504 = 0.03720 0.00926 0.00721 -0.00309 C8 1 0.624288 0.838222 0.214566 11.00000 0.05053 0.04307 = 0.03456 0.00368 0.00497 -0.00589 AFIX 43 H8 2 0.597575 0.799587 0.175219 11.00000 -1.20000 AFIX 0 C9 1 0.700549 0.828013 0.216562 11.00000 0.04845 0.05194 = 0.05109 0.00829 0.01328 -0.00030 AFIX 43 H9 2 0.726286 0.782945 0.178271 11.00000 -1.20000 AFIX 0 C10 1 0.738408 0.882899 0.273679 11.00000 0.04934 0.05628 = 0.06154 0.02178 0.00247 -0.01029 AFIX 43 H10 2 0.790480 0.875401 0.275114 11.00000 -1.20000 AFIX 0 C11 1 0.701138 0.949565 0.329620 11.00000 0.06989 0.05828 = 0.04636 0.00889 -0.00963 -0.02803 AFIX 43 H11 2 0.727677 0.986696 0.369427 11.00000 -1.20000 AFIX 0 C12 1 0.625463 0.961937 0.327426 11.00000 0.06217 0.04992 = 0.03941 -0.00154 0.01053 -0.01439 AFIX 43 H12 2 0.599717 1.009307 0.365030 11.00000 -1.20000 AFIX 0 C13 1 0.226897 0.560187 0.412808 11.00000 0.03002 0.03061 = 0.02785 0.00121 0.00082 -0.00172 C14 1 0.212486 0.485413 0.349775 11.00000 0.03764 0.03498 = 0.03410 -0.00634 -0.00048 -0.00082 AFIX 43 H14 2 0.248505 0.422403 0.329926 11.00000 -1.20000 AFIX 0 C15 1 0.145418 0.503190 0.316069 11.00000 0.04089 0.04547 = 0.03447 -0.00692 -0.00657 -0.00583 AFIX 43 H15 2 0.135676 0.453335 0.272548 11.00000 -1.20000 AFIX 0 C16 1 0.092314 0.593332 0.345411 11.00000 0.03294 0.04673 = 0.04487 0.00094 -0.00862 -0.00296 AFIX 43 H16 2 0.046502 0.606137 0.321811 11.00000 -1.20000 AFIX 0 C17 1 0.106276 0.664588 0.409196 11.00000 0.03534 0.04816 = 0.05153 -0.00913 -0.00359 0.00698 AFIX 43 H17 2 0.069327 0.723780 0.430237 11.00000 -1.20000 AFIX 0 C18 1 0.173716 0.650028 0.442417 11.00000 0.03736 0.04241 = 0.03704 -0.00891 -0.00374 0.00475 AFIX 43 H18 2 0.183662 0.701432 0.485455 11.00000 -1.20000 AFIX 0 C19 1 0.354746 0.372261 0.450703 11.00000 0.03492 0.02938 = 0.02714 -0.00108 -0.00006 -0.00096 C20 1 0.350892 0.285432 0.510913 11.00000 0.07922 0.03721 = 0.03339 0.00376 0.01008 0.01152 AFIX 43 H20 2 0.328463 0.320874 0.553401 11.00000 -1.20000 AFIX 0 C21 1 0.379986 0.146215 0.508899 11.00000 0.11150 0.03727 = 0.03661 0.00952 0.00731 0.01633 AFIX 43 H21 2 0.376555 0.085714 0.549985 11.00000 -1.20000 AFIX 0 C22 1 0.413760 0.094635 0.448128 11.00000 0.06956 0.02882 = 0.04796 -0.00096 -0.00193 0.01144 AFIX 43 H22 2 0.434905 0.000189 0.447913 11.00000 -1.20000 AFIX 0 C23 1 0.416954 0.180112 0.387380 11.00000 0.03875 0.03271 = 0.03701 -0.00437 0.00296 0.00243 AFIX 43 H23 2 0.439199 0.143560 0.345030 11.00000 -1.20000 AFIX 0 C24 1 0.387674 0.319242 0.388278 11.00000 0.03715 0.03156 = 0.02939 -0.00016 0.00085 0.00202 AFIX 43 H24 2 0.389966 0.378375 0.346637 11.00000 -1.20000 AFIX 0 C25 1 0.316870 0.629780 0.539059 11.00000 0.03595 0.03064 = 0.02485 -0.00242 -0.00082 0.00265 C26 1 0.367142 0.736180 0.557785 11.00000 0.03701 0.03051 = 0.03217 -0.00113 -0.00100 0.00279 AFIX 43 H26 2 0.401683 0.770334 0.523542 11.00000 -1.20000 AFIX 0 C27 1 0.367034 0.792781 0.626476 11.00000 0.04711 0.03539 = 0.03459 -0.00549 -0.00657 0.00164 AFIX 43 H27 2 0.402105 0.864508 0.639630 11.00000 -1.20000 AFIX 0 C28 1 0.316126 0.745158 0.675716 11.00000 0.05790 0.04731 = 0.02487 -0.00648 -0.00413 0.00645 AFIX 43 H28 2 0.315587 0.785821 0.722466 11.00000 -1.20000 AFIX 0 C29 1 0.265585 0.638246 0.657636 11.00000 0.05089 0.05374 = 0.02816 -0.00224 0.00528 -0.00260 AFIX 43 H29 2 0.231038 0.605094 0.692111 11.00000 -1.20000 AFIX 0 C30 1 0.265570 0.579683 0.588976 11.00000 0.04025 0.04402 = 0.03060 -0.00194 0.00150 -0.00495 AFIX 43 H30 2 0.231112 0.506539 0.576183 11.00000 -1.20000 AFIX 0 HKLF 4 REM JD_POP_0m in Pca2(1) REM wR2 = 0.0813, GooF = S = 1.092, Restrained GooF = 1.097 for all data REM R1 = 0.0303 for 5354 Fo > 4sig(Fo) and 0.0313 for all 5537 data REM 561 parameters refined using 532 restraints END WGHT 0.0374 0.8833 REM Highest difference peak 0.205, deepest hole -0.288, 1-sigma level 0.038 Q1 1 0.3527 0.3391 0.4165 11.00000 0.05 0.21 Q2 1 0.3213 0.5860 0.5021 11.00000 0.05 0.20 Q3 1 0.3490 0.5685 0.4091 11.00000 0.05 0.19 Q4 1 0.6230 0.6226 0.6272 11.00000 0.05 0.16 Q5 1 0.3857 0.3623 0.4232 11.00000 0.05 0.16 Q6 1 0.3469 0.4281 0.4482 11.00000 0.05 0.16 Q7 1 0.5520 0.9642 0.5005 11.00000 0.05 0.15 Q8 1 0.1085 0.6450 0.3734 11.00000 0.05 0.15 Q9 1 0.3524 0.6431 0.3467 11.00000 0.05 0.15 Q10 1 0.4826 0.4989 0.6705 11.00000 0.05 0.15 Q11 1 0.4885 0.7402 0.3116 11.00000 0.05 0.14 Q12 1 0.6340 0.9982 0.4467 11.00000 0.05 0.14 Q13 1 0.4529 -0.1456 0.4651 11.00000 0.05 0.14 Q14 1 0.3280 0.8248 0.7390 11.00000 0.05 0.14 Q15 1 0.6109 0.6789 0.6275 11.00000 0.05 0.14 Q16 1 0.3524 0.3400 0.4845 11.00000 0.05 0.14 Q17 1 0.2642 0.5636 0.6344 11.00000 0.05 0.14 Q18 1 0.4190 0.1476 0.4215 11.00000 0.05 0.14 Q19 1 0.5999 0.9944 0.5883 11.00000 0.05 0.14 Q20 1 0.3916 0.7320 0.5455 11.00000 0.05 0.14 ; _shelx_res_checksum 81472 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' 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 F1 F 0.58459(16) 0.3767(3) 0.6225(2) 0.0632(8) Uani 0.783(3) 1 d D U P A 1 F2 F 0.4960(2) 0.4331(4) 0.6918(2) 0.0753(10) Uani 0.783(3) 1 d D U P A 1 F3 F 0.49794(18) 0.5119(3) 0.58362(19) 0.0637(8) Uani 0.783(3) 1 d D U P A 1 S1 S 0.58916(16) 0.6423(3) 0.67232(18) 0.0380(5) Uani 0.783(3) 1 d D U P A 1 C31 C 0.5390(4) 0.4818(6) 0.6396(4) 0.0444(12) Uani 0.783(3) 1 d D U P A 1 O2 O 0.5341(2) 0.7405(4) 0.6966(2) 0.0510(8) Uani 0.783(3) 1 d D U P A 1 O3 O 0.63932(19) 0.5830(4) 0.72413(18) 0.0508(8) Uani 0.783(3) 1 d D U P A 1 N1 N 0.63666(18) 0.6904(4) 0.6054(2) 0.0397(7) Uani 0.783(3) 1 d D U P A 1 O4 O 0.53173(16) 0.8184(4) 0.5403(2) 0.0541(8) Uani 0.783(3) 1 d D U P A 1 O5 O 0.6479(2) 0.7622(4) 0.48079(19) 0.0633(9) Uani 0.783(3) 1 d D U P A 1 S2 S 0.6088(2) 0.7962(4) 0.5448(2) 0.0377(5) Uani 0.783(3) 1 d D U P A 1 C32 C 0.6442(5) 0.9730(7) 0.5727(5) 0.0587(14) Uani 0.783(3) 1 d D U P A 1 F4 F 0.6223(3) 1.0085(4) 0.6356(2) 0.0946(14) Uani 0.783(3) 1 d D U P A 1 F5 F 0.6219(3) 1.0724(4) 0.5257(2) 0.0891(13) Uani 0.783(3) 1 d D U P A 1 F6 F 0.7170(2) 0.9738(5) 0.5716(3) 0.0963(13) Uani 0.783(3) 1 d D U P A 1 F1B F 0.5559(7) 0.3872(12) 0.6831(7) 0.075(3) Uani 0.217(3) 1 d D U P A 2 F2B F 0.4679(5) 0.4877(12) 0.6304(7) 0.062(3) Uani 0.217(3) 1 d D U P A 2 F3B F 0.5710(7) 0.4586(12) 0.5759(6) 0.069(3) Uani 0.217(3) 1 d D U P A 2 S1B S 0.5737(6) 0.6685(12) 0.6718(7) 0.043(2) Uani 0.217(3) 1 d D U P A 2 C31B C 0.5407(12) 0.492(2) 0.6377(12) 0.050(3) Uani 0.217(3) 1 d D U P A 2 O2B O 0.5268(8) 0.6953(17) 0.7315(7) 0.065(4) Uani 0.217(3) 1 d D U P A 2 O3B O 0.6498(5) 0.6423(13) 0.6831(7) 0.052(3) Uani 0.217(3) 1 d D U P A 2 N1B N 0.5531(7) 0.7750(13) 0.6077(7) 0.043(2) Uani 0.217(3) 1 d D U P A 2 O4B O 0.5630(8) 0.8619(15) 0.4865(7) 0.068(3) Uani 0.217(3) 1 d D U P A 2 O5B O 0.6685(7) 0.7314(13) 0.5342(8) 0.063(3) Uani 0.217(3) 1 d D U P A 2 S2B S 0.6064(9) 0.8176(17) 0.5453(9) 0.047(2) Uani 0.217(3) 1 d D U P A 2 C32B C 0.6446(13) 0.992(2) 0.5740(16) 0.058(3) Uani 0.217(3) 1 d D U P A 2 F4B F 0.6932(8) 1.0402(12) 0.5297(8) 0.080(3) Uani 0.217(3) 1 d D U P A 2 F5B F 0.5923(9) 1.0911(14) 0.5823(9) 0.093(4) Uani 0.217(3) 1 d D U P A 2 F6B F 0.6760(10) 0.9821(17) 0.6370(9) 0.085(4) Uani 0.217(3) 1 d D U P A 2 P1 P 0.31803(3) 0.55464(6) 0.44999(5) 0.02689(14) Uani 1 1 d . . . . . O1 O 0.51115(12) 0.9148(2) 0.26574(14) 0.0457(5) Uani 1 1 d . . . . . C1 C 0.37628(15) 0.6605(3) 0.39305(15) 0.0281(5) Uani 1 1 d . . . . . C2 C 0.45276(15) 0.6523(3) 0.40201(16) 0.0315(6) Uani 1 1 d . . . . . H2 H 0.472694 0.588693 0.437086 0.038 Uiso 1 1 calc R U . . . C3 C 0.49942(15) 0.7355(3) 0.36045(16) 0.0320(6) Uani 1 1 d . . . . . H3 H 0.551138 0.729938 0.367011 0.038 Uiso 1 1 calc R U . . . C4 C 0.46971(16) 0.8277(3) 0.30877(16) 0.0326(6) Uani 1 1 d . . . . . C5 C 0.39417(17) 0.8362(3) 0.29923(17) 0.0351(6) Uani 1 1 d . . . . . H5 H 0.374426 0.898853 0.263675 0.042 Uiso 1 1 calc R U . . . C6 C 0.34755(15) 0.7537(3) 0.34125(16) 0.0317(6) Uani 1 1 d . . . . . H6 H 0.295851 0.760596 0.334850 0.038 Uiso 1 1 calc R U . . . C7 C 0.58800(17) 0.9048(3) 0.27016(18) 0.0391(7) Uani 1 1 d . . . . . C8 C 0.62429(19) 0.8382(3) 0.21457(18) 0.0427(7) Uani 1 1 d . . . . . H8 H 0.597575 0.799587 0.175219 0.051 Uiso 1 1 calc R U . . . C9 C 0.7005(2) 0.8280(4) 0.2166(2) 0.0505(8) Uani 1 1 d . . . . . H9 H 0.726286 0.782945 0.178271 0.061 Uiso 1 1 calc R U . . . C10 C 0.7384(2) 0.8829(4) 0.2737(2) 0.0557(9) Uani 1 1 d . . . . . H10 H 0.790480 0.875401 0.275114 0.067 Uiso 1 1 calc R U . . . C11 C 0.7011(3) 0.9496(4) 0.3296(2) 0.0582(10) Uani 1 1 d . . . . . H11 H 0.727677 0.986696 0.369427 0.070 Uiso 1 1 calc R U . . . C12 C 0.6255(2) 0.9619(4) 0.3274(2) 0.0505(8) Uani 1 1 d . . . . . H12 H 0.599717 1.009307 0.365030 0.061 Uiso 1 1 calc R U . . . C13 C 0.22690(15) 0.5602(3) 0.41281(15) 0.0295(5) Uani 1 1 d . . . . . C14 C 0.21249(16) 0.4854(3) 0.34978(17) 0.0356(6) Uani 1 1 d . . . . . H14 H 0.248505 0.422403 0.329926 0.043 Uiso 1 1 calc R U . . . C15 C 0.14542(18) 0.5032(3) 0.31607(18) 0.0403(7) Uani 1 1 d . . . . . H15 H 0.135676 0.453335 0.272548 0.048 Uiso 1 1 calc R U . . . C16 C 0.09231(16) 0.5933(3) 0.34541(19) 0.0415(7) Uani 1 1 d . . . . . H16 H 0.046502 0.606137 0.321811 0.050 Uiso 1 1 calc R U . . . C17 C 0.10628(18) 0.6646(4) 0.4092(2) 0.0450(8) Uani 1 1 d . . . . . H17 H 0.069327 0.723780 0.430237 0.054 Uiso 1 1 calc R U . . . C18 C 0.17372(16) 0.6500(3) 0.44242(19) 0.0389(6) Uani 1 1 d . . . . . H18 H 0.183662 0.701432 0.485455 0.047 Uiso 1 1 calc R U . . . C19 C 0.35475(14) 0.3723(3) 0.45070(16) 0.0305(5) Uani 1 1 d . . . . . C20 C 0.3509(2) 0.2854(4) 0.51091(19) 0.0499(9) Uani 1 1 d . . . . . H20 H 0.328463 0.320874 0.553401 0.060 Uiso 1 1 calc R U . . . C21 C 0.3800(3) 0.1462(4) 0.5089(2) 0.0618(11) Uani 1 1 d . . . . . H21 H 0.376555 0.085714 0.549985 0.074 Uiso 1 1 calc R U . . . C22 C 0.4138(2) 0.0946(3) 0.4481(2) 0.0488(8) Uani 1 1 d . . . . . H22 H 0.434905 0.000189 0.447913 0.059 Uiso 1 1 calc R U . . . C23 C 0.41695(16) 0.1801(3) 0.38738(18) 0.0362(6) Uani 1 1 d . . . . . H23 H 0.439199 0.143560 0.345030 0.043 Uiso 1 1 calc R U . . . C24 C 0.38767(16) 0.3192(3) 0.38828(17) 0.0327(6) Uani 1 1 d . . . . . H24 H 0.389966 0.378375 0.346637 0.039 Uiso 1 1 calc R U . . . C25 C 0.31687(15) 0.6298(3) 0.53906(16) 0.0305(5) Uani 1 1 d . . . . . C26 C 0.36714(16) 0.7362(3) 0.55778(16) 0.0332(6) Uani 1 1 d . . . . . H26 H 0.401683 0.770334 0.523542 0.040 Uiso 1 1 calc R U . . . C27 C 0.36703(18) 0.7928(3) 0.62648(17) 0.0390(7) Uani 1 1 d . . . . . H27 H 0.402105 0.864508 0.639630 0.047 Uiso 1 1 calc R U . . . C28 C 0.31613(19) 0.7452(3) 0.67572(18) 0.0434(7) Uani 1 1 d . . . . . H28 H 0.315587 0.785821 0.722466 0.052 Uiso 1 1 calc R U . . . C29 C 0.26558(19) 0.6382(4) 0.65764(17) 0.0443(7) Uani 1 1 d . . . . . H29 H 0.231038 0.605094 0.692111 0.053 Uiso 1 1 calc R U . . . C30 C 0.26557(17) 0.5797(3) 0.58898(17) 0.0383(6) Uani 1 1 d . . . . . H30 H 0.231112 0.506539 0.576183 0.046 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 F1 0.0630(18) 0.0431(14) 0.083(2) -0.0073(15) -0.0024(16) 0.0039(12) F2 0.077(2) 0.0718(19) 0.077(2) 0.0169(17) 0.0304(19) -0.0187(16) F3 0.070(2) 0.0532(15) 0.068(2) 0.0074(15) -0.0278(17) -0.0125(13) S1 0.0475(11) 0.0403(9) 0.0262(7) 0.0021(6) 0.0038(7) 0.0015(6) C31 0.047(2) 0.042(2) 0.044(2) 0.009(2) 0.003(2) -0.001(2) O2 0.059(2) 0.0487(18) 0.045(2) -0.0026(16) 0.0120(17) 0.0130(16) O3 0.064(2) 0.0554(17) 0.0332(16) 0.0059(14) -0.0066(15) 0.0034(15) N1 0.0395(16) 0.0423(16) 0.0372(18) 0.0032(14) -0.0003(14) -0.0010(13) O4 0.0432(16) 0.0636(18) 0.056(2) 0.0198(17) -0.0111(16) -0.0062(14) O5 0.082(2) 0.073(2) 0.0348(18) 0.0045(17) 0.0078(17) -0.0013(19) S2 0.0435(9) 0.0434(11) 0.0262(9) 0.0021(8) -0.0032(7) -0.0080(7) C32 0.076(3) 0.051(3) 0.049(3) 0.015(3) -0.013(3) -0.015(3) F4 0.173(5) 0.0537(19) 0.057(2) -0.0149(17) 0.005(3) -0.019(3) F5 0.130(3) 0.0514(17) 0.086(3) 0.0330(18) -0.034(3) -0.0246(19) F6 0.080(2) 0.102(3) 0.107(3) 0.016(3) -0.032(2) -0.046(2) F1B 0.079(7) 0.062(6) 0.082(8) 0.043(6) -0.010(6) -0.002(5) F2B 0.039(5) 0.064(5) 0.084(7) 0.020(6) -0.009(5) -0.010(4) F3B 0.087(7) 0.057(5) 0.063(6) -0.007(5) 0.011(6) -0.011(5) S1B 0.053(4) 0.050(4) 0.027(2) 0.006(3) -0.001(3) -0.007(3) C31B 0.053(6) 0.050(6) 0.046(6) 0.011(6) 0.002(6) 0.002(6) O2B 0.081(8) 0.074(8) 0.040(7) 0.008(6) 0.012(6) -0.015(7) O3B 0.027(5) 0.069(6) 0.061(7) 0.019(6) -0.014(5) -0.007(4) N1B 0.044(4) 0.047(4) 0.038(4) 0.004(4) -0.002(4) -0.005(4) O4B 0.086(8) 0.080(7) 0.038(6) 0.013(6) -0.018(6) -0.028(6) O5B 0.074(7) 0.055(6) 0.060(8) 0.010(6) 0.033(6) 0.009(5) S2B 0.061(4) 0.050(4) 0.031(4) 0.018(3) -0.003(3) -0.010(3) C32B 0.078(6) 0.046(6) 0.050(6) 0.009(6) -0.014(6) -0.019(6) F4B 0.095(8) 0.059(6) 0.086(8) 0.035(6) -0.006(7) -0.030(6) F5B 0.135(9) 0.057(6) 0.086(8) 0.000(6) -0.008(8) 0.027(6) F6B 0.105(9) 0.074(7) 0.076(8) -0.005(6) -0.030(8) -0.029(7) P1 0.0303(3) 0.0279(3) 0.0225(3) -0.0014(3) 0.0001(3) 0.0008(2) O1 0.0428(11) 0.0464(11) 0.0479(14) 0.0191(11) 0.0107(10) 0.0037(9) C1 0.0316(13) 0.0279(11) 0.0248(13) -0.0024(10) 0.0014(11) 0.0016(9) C2 0.0338(14) 0.0314(12) 0.0291(14) 0.0021(11) 0.0004(11) 0.0033(10) C3 0.0316(12) 0.0323(12) 0.0322(15) 0.0004(11) 0.0046(12) 0.0005(10) C4 0.0405(15) 0.0288(12) 0.0285(14) 0.0010(11) 0.0090(12) 0.0007(10) C5 0.0410(15) 0.0347(13) 0.0297(15) 0.0049(12) 0.0002(12) 0.0054(11) C6 0.0336(13) 0.0333(13) 0.0281(14) -0.0006(11) -0.0006(11) 0.0044(10) C7 0.0452(16) 0.0350(14) 0.0372(16) 0.0093(12) 0.0072(13) -0.0031(12) C8 0.0505(18) 0.0431(15) 0.0346(17) 0.0037(13) 0.0050(14) -0.0059(13) C9 0.0484(19) 0.0519(18) 0.051(2) 0.0083(16) 0.0133(16) -0.0003(15) C10 0.0493(19) 0.0563(19) 0.062(2) 0.0218(18) 0.0025(18) -0.0103(16) C11 0.070(2) 0.058(2) 0.046(2) 0.0089(17) -0.0096(19) -0.0280(19) C12 0.062(2) 0.0499(18) 0.0394(19) -0.0015(15) 0.0105(17) -0.0144(16) C13 0.0300(12) 0.0306(12) 0.0278(14) 0.0012(10) 0.0008(11) -0.0017(9) C14 0.0376(14) 0.0350(13) 0.0341(15) -0.0063(12) -0.0005(12) -0.0008(11) C15 0.0409(16) 0.0455(16) 0.0345(16) -0.0069(13) -0.0066(13) -0.0058(13) C16 0.0329(14) 0.0467(16) 0.0449(19) 0.0009(14) -0.0086(13) -0.0030(12) C17 0.0353(16) 0.0482(17) 0.052(2) -0.0091(15) -0.0036(14) 0.0070(12) C18 0.0374(14) 0.0424(14) 0.0370(16) -0.0089(13) -0.0037(13) 0.0048(11) C19 0.0349(12) 0.0294(11) 0.0271(13) -0.0011(11) -0.0001(12) -0.0010(9) C20 0.079(3) 0.0372(15) 0.0334(17) 0.0038(13) 0.0101(17) 0.0115(15) C21 0.112(3) 0.0373(16) 0.0366(19) 0.0095(14) 0.007(2) 0.0163(19) C22 0.070(2) 0.0288(13) 0.0480(19) -0.0010(14) -0.0019(18) 0.0114(13) C23 0.0387(15) 0.0327(13) 0.0370(16) -0.0044(12) 0.0030(13) 0.0024(11) C24 0.0371(14) 0.0316(13) 0.0294(14) -0.0002(11) 0.0009(12) 0.0020(11) C25 0.0360(13) 0.0306(12) 0.0248(13) -0.0024(11) -0.0008(11) 0.0027(9) C26 0.0370(14) 0.0305(12) 0.0322(15) -0.0011(11) -0.0010(12) 0.0028(10) C27 0.0471(17) 0.0354(14) 0.0346(17) -0.0055(12) -0.0066(13) 0.0016(12) C28 0.0579(18) 0.0473(16) 0.0249(14) -0.0065(14) -0.0041(13) 0.0064(13) C29 0.0509(18) 0.0537(18) 0.0282(16) -0.0022(13) 0.0053(14) -0.0026(14) C30 0.0403(16) 0.0440(15) 0.0306(15) -0.0019(12) 0.0015(12) -0.0050(12) 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' 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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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_ _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 O2 S1 O3 118.2(3) . . ? O2 S1 N1 117.3(3) . . ? O3 S1 N1 106.9(3) . . ? O2 S1 C31 105.4(3) . . ? O3 S1 C31 103.5(3) . . ? N1 S1 C31 103.4(3) . . ? F1 C31 F3 108.7(5) . . ? F1 C31 F2 107.5(5) . . ? F3 C31 F2 108.7(5) . . ? F1 C31 S1 111.0(4) . . ? F3 C31 S1 112.2(4) . . ? F2 C31 S1 108.6(4) . . ? S2 N1 S1 124.3(3) . . ? O4 S2 O5 118.3(4) . . ? O4 S2 N1 116.7(3) . . ? O5 S2 N1 107.8(3) . . ? O4 S2 C32 103.8(4) . . ? O5 S2 C32 105.0(4) . . ? N1 S2 C32 103.4(3) . . ? F4 C32 F6 108.9(6) . . ? F4 C32 F5 109.6(7) . . ? F6 C32 F5 106.9(7) . . ? F4 C32 S2 112.2(6) . . ? F6 C32 S2 110.7(5) . . ? F5 C32 S2 108.4(5) . . ? O3B S1B O2B 119.8(13) . . ? O3B S1B N1B 116.4(10) . . ? O2B S1B N1B 109.9(10) . . ? O3B S1B C31B 102.7(10) . . ? O2B S1B C31B 103.2(11) . . ? N1B S1B C31B 101.9(10) . . ? F1B C31B F3B 108.0(17) . . ? F1B C31B F2B 104.8(16) . . ? F3B C31B F2B 108.8(17) . . ? F1B C31B S1B 110.7(14) . . ? F3B C31B S1B 111.8(14) . . ? F2B C31B S1B 112.5(14) . . ? S2B N1B S1B 124.7(11) . . ? O5B S2B O4B 120.1(15) . . ? O5B S2B N1B 118.0(12) . . ? O4B S2B N1B 107.8(12) . . ? O5B S2B C32B 103.5(13) . . ? O4B S2B C32B 100.8(12) . . ? N1B S2B C32B 103.6(13) . . ? F4B C32B F6B 107.5(18) . . ? F4B C32B F5B 109.1(19) . . ? F6B C32B F5B 105(2) . . ? F4B C32B S2B 112.1(18) . . ? F6B C32B S2B 111.7(16) . . ? F5B C32B S2B 111.4(15) . . ? C1 P1 C13 107.51(13) . . ? C1 P1 C25 110.32(13) . . ? C13 P1 C25 109.57(13) . . ? C1 P1 C19 106.91(12) . . ? C13 P1 C19 111.72(12) . . ? C25 P1 C19 110.73(13) . . ? C4 O1 C7 118.6(2) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 P1 121.7(2) . . ? C2 C1 P1 119.1(2) . . ? C3 C2 C1 120.8(3) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? O1 C4 C5 116.0(3) . . ? O1 C4 C3 123.5(3) . . ? C5 C4 C3 120.5(3) . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 120.1(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 121.4(3) . . ? C12 C7 O1 121.0(3) . . ? C8 C7 O1 117.6(3) . . ? C7 C8 C9 119.3(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C7 C12 C11 119.1(4) . . ? C7 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C18 C13 C14 120.1(3) . . ? C18 C13 P1 120.4(2) . . ? C14 C13 P1 119.2(2) . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.4(3) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 119.9(3) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? C20 C19 C24 119.9(3) . . ? C20 C19 P1 121.6(2) . . ? C24 C19 P1 118.4(2) . . ? C19 C20 C21 119.5(3) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.8(3) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 119.8(3) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C26 C25 C30 120.4(3) . . ? C26 C25 P1 119.8(2) . . ? C30 C25 P1 119.8(2) . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C29 120.6(3) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 119.2(3) . . ? C29 C30 H30 120.4 . . ? C25 C30 H30 120.4 . . ? 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 F1 C31 1.313(7) . ? F2 C31 1.328(7) . ? F3 C31 1.314(7) . ? S1 O2 1.422(3) . ? S1 O3 1.437(4) . ? S1 N1 1.582(5) . ? S1 C31 1.840(6) . ? N1 S2 1.577(5) . ? O4 S2 1.419(5) . ? O5 S2 1.426(5) . ? S2 C32 1.825(6) . ? C32 F4 1.283(11) . ? C32 F6 1.324(9) . ? C32 F5 1.331(8) . ? F1B C31B 1.31(2) . ? F2B C31B 1.33(2) . ? F3B C31B 1.32(2) . ? S1B O3B 1.421(12) . ? S1B O2B 1.426(15) . ? S1B N1B 1.592(14) . ? S1B C31B 1.846(18) . ? N1B S2B 1.566(17) . ? O4B S2B 1.412(17) . ? O5B S2B 1.396(16) . ? S2B C32B 1.826(18) . ? C32B F4B 1.29(3) . ? C32B F6B 1.31(2) . ? C32B F5B 1.33(2) . ? P1 C1 1.789(3) . ? P1 C13 1.798(3) . ? P1 C25 1.802(3) . ? P1 C19 1.806(3) . ? O1 C4 1.362(3) . ? O1 C7 1.403(4) . ? C1 C6 1.394(4) . ? C1 C2 1.403(4) . ? C2 C3 1.382(4) . ? C2 H2 0.9500 . ? C3 C4 1.394(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C5 C6 1.382(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.373(5) . ? C7 C8 1.375(5) . ? C8 C9 1.391(5) . ? C8 H8 0.9500 . ? C9 C10 1.366(6) . ? C9 H9 0.9500 . ? C10 C11 1.388(6) . ? C10 H10 0.9500 . ? C11 C12 1.382(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.387(4) . ? C13 C14 1.388(4) . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.381(4) . ? C19 C24 1.399(4) . ? C20 C21 1.386(5) . ? C20 H20 0.9500 . ? C21 C22 1.375(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.384(4) . ? C25 C30 1.397(4) . ? C26 C27 1.385(4) . ? C26 H26 0.9500 . ? C27 C28 1.377(5) . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 C30 1.391(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 C31 F1 -173.4(5) . . . . ? O3 S1 C31 F1 -48.6(5) . . . . ? N1 S1 C31 F1 62.9(5) . . . . ? O2 S1 C31 F3 64.8(5) . . . . ? O3 S1 C31 F3 -170.4(4) . . . . ? N1 S1 C31 F3 -59.0(5) . . . . ? O2 S1 C31 F2 -55.3(5) . . . . ? O3 S1 C31 F2 69.5(5) . . . . ? N1 S1 C31 F2 -179.1(4) . . . . ? O2 S1 N1 S2 -28.0(5) . . . . ? O3 S1 N1 S2 -163.5(3) . . . . ? C31 S1 N1 S2 87.6(4) . . . . ? S1 N1 S2 O4 -17.1(5) . . . . ? S1 N1 S2 O5 -153.0(3) . . . . ? S1 N1 S2 C32 96.1(5) . . . . ? O4 S2 C32 F4 65.1(6) . . . . ? O5 S2 C32 F4 -170.1(5) . . . . ? N1 S2 C32 F4 -57.2(6) . . . . ? O4 S2 C32 F6 -173.0(6) . . . . ? O5 S2 C32 F6 -48.2(7) . . . . ? N1 S2 C32 F6 64.7(7) . . . . ? O4 S2 C32 F5 -56.1(7) . . . . ? O5 S2 C32 F5 68.7(7) . . . . ? N1 S2 C32 F5 -178.4(6) . . . . ? O3B S1B C31B F1B 56.6(18) . . . . ? O2B S1B C31B F1B -68.6(18) . . . . ? N1B S1B C31B F1B 177.4(15) . . . . ? O3B S1B C31B F3B -63.8(18) . . . . ? O2B S1B C31B F3B 171.0(15) . . . . ? N1B S1B C31B F3B 57.0(17) . . . . ? O3B S1B C31B F2B 173.5(15) . . . . ? O2B S1B C31B F2B 48.3(18) . . . . ? N1B S1B C31B F2B -65.7(17) . . . . ? O3B S1B N1B S2B 17.4(18) . . . . ? O2B S1B N1B S2B 157.7(13) . . . . ? C31B S1B N1B S2B -93.3(14) . . . . ? S1B N1B S2B O5B 17(2) . . . . ? S1B N1B S2B O4B 156.9(12) . . . . ? S1B N1B S2B C32B -96.8(14) . . . . ? O5B S2B C32B F4B 53.1(19) . . . . ? O4B S2B C32B F4B -71.7(19) . . . . ? N1B S2B C32B F4B 176.8(16) . . . . ? O5B S2B C32B F6B -68(2) . . . . ? O4B S2B C32B F6B 168(2) . . . . ? N1B S2B C32B F6B 56(2) . . . . ? O5B S2B C32B F5B 175.7(19) . . . . ? O4B S2B C32B F5B 51(2) . . . . ? N1B S2B C32B F5B -61(2) . . . . ? C13 P1 C1 C6 13.6(3) . . . . ? C25 P1 C1 C6 -105.8(2) . . . . ? C19 P1 C1 C6 133.7(2) . . . . ? C13 P1 C1 C2 -168.1(2) . . . . ? C25 P1 C1 C2 72.5(2) . . . . ? C19 P1 C1 C2 -48.0(2) . . . . ? C6 C1 C2 C3 0.2(4) . . . . ? P1 C1 C2 C3 -178.1(2) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? C7 O1 C4 C5 -176.4(3) . . . . ? C7 O1 C4 C3 4.3(4) . . . . ? C2 C3 C4 O1 179.4(3) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? O1 C4 C5 C6 -178.9(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C1 -0.6(4) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? P1 C1 C6 C5 178.6(2) . . . . ? C4 O1 C7 C12 -74.1(4) . . . . ? C4 O1 C7 C8 107.0(3) . . . . ? C12 C7 C8 C9 0.3(5) . . . . ? O1 C7 C8 C9 179.2(3) . . . . ? C7 C8 C9 C10 0.5(5) . . . . ? C8 C9 C10 C11 -0.3(5) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C8 C7 C12 C11 -1.2(5) . . . . ? O1 C7 C12 C11 179.9(3) . . . . ? C10 C11 C12 C7 1.4(5) . . . . ? C1 P1 C13 C18 -102.2(3) . . . . ? C25 P1 C13 C18 17.7(3) . . . . ? C19 P1 C13 C18 140.8(2) . . . . ? C1 P1 C13 C14 71.1(2) . . . . ? C25 P1 C13 C14 -169.0(2) . . . . ? C19 P1 C13 C14 -45.9(3) . . . . ? C18 C13 C14 C15 1.2(4) . . . . ? P1 C13 C14 C15 -172.1(2) . . . . ? C13 C14 C15 C16 -1.0(5) . . . . ? C14 C15 C16 C17 -0.7(5) . . . . ? C15 C16 C17 C18 2.2(5) . . . . ? C16 C17 C18 C13 -1.9(5) . . . . ? C14 C13 C18 C17 0.2(5) . . . . ? P1 C13 C18 C17 173.5(3) . . . . ? C1 P1 C19 C20 146.1(3) . . . . ? C13 P1 C19 C20 -96.5(3) . . . . ? C25 P1 C19 C20 25.9(3) . . . . ? C1 P1 C19 C24 -33.9(3) . . . . ? C13 P1 C19 C24 83.4(2) . . . . ? C25 P1 C19 C24 -154.1(2) . . . . ? C24 C19 C20 C21 0.2(6) . . . . ? P1 C19 C20 C21 -179.9(3) . . . . ? C19 C20 C21 C22 1.2(7) . . . . ? C20 C21 C22 C23 -2.1(7) . . . . ? C21 C22 C23 C24 1.6(5) . . . . ? C22 C23 C24 C19 -0.2(5) . . . . ? C20 C19 C24 C23 -0.6(5) . . . . ? P1 C19 C24 C23 179.4(2) . . . . ? C1 P1 C25 C26 -11.3(3) . . . . ? C13 P1 C25 C26 -129.5(2) . . . . ? C19 P1 C25 C26 106.8(2) . . . . ? C1 P1 C25 C30 169.1(2) . . . . ? C13 P1 C25 C30 50.9(3) . . . . ? C19 P1 C25 C30 -72.8(3) . . . . ? C30 C25 C26 C27 0.4(4) . . . . ? P1 C25 C26 C27 -179.1(2) . . . . ? C25 C26 C27 C28 -1.2(4) . . . . ? C26 C27 C28 C29 1.4(5) . . . . ? C27 C28 C29 C30 -0.8(5) . . . . ? C28 C29 C30 C25 0.1(5) . . . . ? C26 C25 C30 C29 0.1(4) . . . . ? P1 C25 C30 C29 179.7(2) . . . . ?