#------------------------------------------------------------------------------ #$Date: 2020-05-19 04:38:53 +0300 (Tue, 19 May 2020) $ #$Revision: 252160 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240550.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_7240550 loop_ _publ_author_name 'Suslonov, Vitalii V.' 'Eliseeva, Anastasiya A.' 'Novikov, Alexander S.' 'Ivanov, Daniil M.' 'Dubovtsev, Alexey Yu.' 'Bokach, Nadezhda A.' 'Kukushkin, Vadim Yu.' _publ_section_title ; Tetrachloroplatinate(II) Anion as a Square-planar Tecton for Crystal Engineering Involving Halogen Bonding ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00576B _journal_year 2020 _chemical_formula_moiety 'C19 H17 I P, C F3 O3 S' _chemical_formula_sum 'C20 H17 F3 I O3 P S' _chemical_formula_weight 552.26 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-02-21 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-03-10 deposited with the CCDC. 2020-05-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.894(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4024(3) _cell_length_b 15.8557(5) _cell_length_c 12.7928(4) _cell_measurement_reflns_used 4274 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.7490 _cell_measurement_theta_min 3.0230 _cell_volume 2090.02(11) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 16.2096 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -87.00 -15.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -25.4311 -57.0000 120.0000 72 #__ type_ start__ end____ width___ exp.time_ 2 omega -96.00 -35.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -25.4311 -178.0000 150.0000 61 #__ type_ start__ end____ width___ exp.time_ 3 omega -40.00 52.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 26.5248 -38.0000 0.0000 92 #__ type_ start__ end____ width___ exp.time_ 4 omega 0.00 32.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 26.5248 -38.0000 -90.0000 32 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0205178000 _diffrn_orient_matrix_UB_12 -0.0267505000 _diffrn_orient_matrix_UB_13 -0.0389371000 _diffrn_orient_matrix_UB_21 -0.0615897000 _diffrn_orient_matrix_UB_22 -0.0200783000 _diffrn_orient_matrix_UB_23 -0.0067764000 _diffrn_orient_matrix_UB_31 -0.0230191000 _diffrn_orient_matrix_UB_32 0.0297078000 _diffrn_orient_matrix_UB_33 -0.0395941000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10364 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 3.003 _diffrn_source 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.754 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.83310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.755 _exptl_crystal_description prism _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.439 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 4806 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0258 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.3655P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.0591 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4172 _reflns_number_total 4806 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00576b2.cif _cod_data_source_block Ph3PCH2I_OTf _cod_original_cell_volume 2090.02(10) _cod_database_code 7240550 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C20 C17 P I F3 S O3' _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_max 0.779 _shelx_estimated_absorpt_t_min 0.721 _reflns_odcompleteness_completeness 99.84 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19) ; _shelx_res_file ; 10622-13266_svv015.res created by SHELXL-2014/7 TITL CF solution in P21/n CELL 0.71073 10.402394 15.855692 12.792825 90 97.8935 90 ZERR 4 0.000278 0.000453 0.000367 0 0.0024 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F I O P S UNIT 80 68 12 4 12 4 4 L.S. 4 PLAN 25 SIZE 0.2 0.15 0.2 TEMP -173(2) BOND fmap 2 acta OMIT -4 55 REM REM REM WGHT 0.023200 0.365500 FVAR 3.27342 I1 4 0.724165 0.718176 0.977885 11.00000 0.01206 0.02655 = 0.02383 0.00283 -0.00293 -0.00427 P1 6 0.423732 0.708506 0.858892 11.00000 0.00974 0.01110 = 0.00920 -0.00031 0.00133 -0.00113 C1 1 0.539466 0.656645 0.955159 11.00000 0.01075 0.01420 = 0.01317 0.00039 -0.00100 -0.00257 AFIX 23 H1A 2 0.551120 0.597824 0.932260 11.00000 -1.20000 H1B 2 0.504584 0.654676 1.023330 11.00000 -1.20000 AFIX 0 C2 1 0.269995 0.656445 0.860303 11.00000 0.01013 0.01325 = 0.01189 -0.00225 0.00285 -0.00234 C3 1 0.260588 0.579387 0.911431 11.00000 0.01315 0.01560 = 0.01241 -0.00039 0.00121 -0.00022 AFIX 43 H3 2 0.336412 0.551567 0.944311 11.00000 -1.20000 AFIX 0 C4 1 0.138915 0.543913 0.913608 11.00000 0.02191 0.01608 = 0.01538 0.00054 0.00329 -0.00585 AFIX 43 H4 2 0.131593 0.491308 0.947846 11.00000 -1.20000 AFIX 0 C5 1 0.027932 0.584672 0.866184 11.00000 0.01468 0.02280 = 0.01667 -0.00465 0.00447 -0.00645 AFIX 43 H5 2 -0.054878 0.560178 0.868950 11.00000 -1.20000 AFIX 0 C6 1 0.037301 0.660944 0.814797 11.00000 0.01274 0.02151 = 0.01625 -0.00065 0.00046 -0.00028 AFIX 43 H6 2 -0.038896 0.688275 0.781781 11.00000 -1.20000 AFIX 0 C7 1 0.157918 0.697340 0.811592 11.00000 0.01346 0.01509 = 0.01470 0.00075 0.00113 -0.00194 AFIX 43 H7 2 0.164622 0.749680 0.776604 11.00000 -1.20000 AFIX 0 C8 1 0.472762 0.700443 0.730253 11.00000 0.01108 0.01399 = 0.01010 0.00112 0.00074 0.00041 C9 1 0.426933 0.633038 0.665734 11.00000 0.01002 0.01339 = 0.01447 0.00093 -0.00091 -0.00137 AFIX 43 H9 2 0.367292 0.593931 0.688360 11.00000 -1.20000 AFIX 0 C10 1 0.469272 0.623573 0.568052 11.00000 0.01440 0.01495 = 0.01417 -0.00364 -0.00202 0.00250 AFIX 43 H10 2 0.438801 0.577553 0.523918 11.00000 -1.20000 AFIX 0 C11 1 0.555561 0.680733 0.534563 11.00000 0.01940 0.02200 = 0.01399 0.00054 0.00449 0.00343 AFIX 43 H11 2 0.582647 0.674482 0.467028 11.00000 -1.20000 AFIX 0 C12 1 0.602615 0.747206 0.599517 11.00000 0.02146 0.01932 = 0.02124 0.00094 0.00902 -0.00414 AFIX 43 H12 2 0.662765 0.785870 0.576719 11.00000 -1.20000 AFIX 0 C13 1 0.561957 0.757272 0.697649 11.00000 0.01878 0.01639 = 0.01545 -0.00257 0.00470 -0.00459 AFIX 43 H13 2 0.594536 0.802483 0.742351 11.00000 -1.20000 AFIX 0 C14 1 0.402653 0.816166 0.896429 11.00000 0.00800 0.01143 = 0.01599 -0.00173 0.00211 -0.00189 C15 1 0.401722 0.832927 1.003481 11.00000 0.01554 0.01609 = 0.01412 0.00074 0.00350 -0.00110 AFIX 43 H15 2 0.420673 0.789536 1.054479 11.00000 -1.20000 AFIX 0 C16 1 0.372719 0.913874 1.034347 11.00000 0.01863 0.02117 = 0.01466 -0.00547 0.00536 -0.00106 AFIX 43 H16 2 0.372071 0.925832 1.107039 11.00000 -1.20000 AFIX 0 C17 1 0.344862 0.977083 0.960820 11.00000 0.01510 0.01640 = 0.02672 -0.00441 0.00614 0.00009 AFIX 43 H17 2 0.324632 1.032126 0.982952 11.00000 -1.20000 AFIX 0 C18 1 0.346309 0.960462 0.854452 11.00000 0.01732 0.01739 = 0.02235 0.00406 0.00215 0.00281 AFIX 43 H18 2 0.327848 1.004248 0.803930 11.00000 -1.20000 AFIX 0 C19 1 0.374776 0.879731 0.821813 11.00000 0.01721 0.01775 = 0.01503 -0.00080 0.00259 -0.00116 AFIX 43 H19 2 0.375180 0.868073 0.749017 11.00000 -1.20000 AFIX 0 S1A 7 0.542054 0.416993 0.778799 11.00000 0.01492 0.01215 = 0.01328 -0.00126 0.00303 -0.00196 F1A 3 0.792063 0.439008 0.837202 11.00000 0.01813 0.02440 = 0.02638 0.00419 -0.00675 -0.00216 F2A 3 0.701103 0.537893 0.737851 11.00000 0.02300 0.01669 = 0.03879 0.01087 0.00561 -0.00288 F3A 3 0.740116 0.417220 0.670459 11.00000 0.02531 0.03634 = 0.02238 0.00012 0.01329 0.00489 O1A 5 0.462982 0.426732 0.678759 11.00000 0.02008 0.02629 = 0.02060 -0.00224 -0.00349 -0.00151 O2A 5 0.567689 0.330973 0.813496 11.00000 0.02720 0.01008 = 0.02191 0.00016 0.00702 -0.00214 O3A 5 0.512129 0.473033 0.861155 11.00000 0.02675 0.01682 = 0.01928 -0.00327 0.01000 0.00046 C1A 1 0.701156 0.454596 0.754229 11.00000 0.01705 0.01466 = 0.01581 0.00321 0.00164 0.00154 HKLF 4 REM CF solution in P21/n REM R1 = 0.0258 for 4172 Fo > 4sig(Fo) and 0.0320 for all 4806 data REM 262 parameters refined using 0 restraints END WGHT 0.0232 0.3655 REM Highest difference peak 0.439, deepest hole -0.551, 1-sigma level 0.088 Q1 1 0.4607 0.7064 0.7866 11.00000 0.05 0.44 Q2 1 0.6229 0.4415 0.7618 11.00000 0.05 0.40 Q3 1 0.4178 0.6439 0.6003 11.00000 0.05 0.39 Q4 1 0.1016 0.6703 0.8009 11.00000 0.05 0.39 Q5 1 0.4150 0.7779 0.8803 11.00000 0.05 0.38 Q6 1 0.2167 0.6629 0.8177 11.00000 0.05 0.37 Q7 1 0.2595 0.6166 0.8786 11.00000 0.05 0.36 Q8 1 0.3109 0.9608 0.9036 11.00000 0.05 0.33 Q9 1 0.3765 0.9251 0.8446 11.00000 0.05 0.32 Q10 1 0.3854 0.9720 0.9152 11.00000 0.05 0.32 Q11 1 0.4144 0.8788 1.0204 11.00000 0.05 0.31 Q12 1 0.3619 1.0491 1.0152 11.00000 0.05 0.31 Q13 1 0.4736 0.6712 0.9050 11.00000 0.05 0.30 Q14 1 0.2804 1.0693 0.9009 11.00000 0.05 0.30 Q15 1 0.3594 0.8209 0.9376 11.00000 0.05 0.29 Q16 1 0.4877 0.5325 0.7603 11.00000 0.05 0.29 Q17 1 0.1779 0.8003 0.7973 11.00000 0.05 0.29 Q18 1 0.5294 0.7219 0.7108 11.00000 0.05 0.29 Q19 1 0.4369 0.6757 0.6773 11.00000 0.05 0.28 Q20 1 0.4668 0.6609 0.7137 11.00000 0.05 0.28 Q21 1 0.2999 0.8671 0.7244 11.00000 0.05 0.28 Q22 1 0.2107 0.6809 0.8531 11.00000 0.05 0.28 Q23 1 0.8265 0.4658 0.6572 11.00000 0.05 0.27 Q24 1 0.5672 0.8098 0.8757 11.00000 0.05 0.27 Q25 1 0.4471 0.6073 0.5415 11.00000 0.05 0.27 ; _shelx_res_checksum 13467 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, 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 I1 I 0.72417(2) 0.71818(2) 0.97788(2) 0.02132(6) Uani 1 1 d . . . . . P1 P 0.42373(5) 0.70851(3) 0.85889(4) 0.01001(11) Uani 1 1 d . . . . . C1 C 0.5395(2) 0.65664(14) 0.95516(16) 0.0130(4) Uani 1 1 d . . . . . H1A H 0.5511 0.5978 0.9323 0.016 Uiso 1 1 calc R . . . . H1B H 0.5046 0.6547 1.0233 0.016 Uiso 1 1 calc R . . . . C2 C 0.2700(2) 0.65644(13) 0.86030(16) 0.0116(4) Uani 1 1 d . . . . . C3 C 0.2606(2) 0.57939(14) 0.91143(16) 0.0138(4) Uani 1 1 d . . . . . H3 H 0.3364 0.5516 0.9443 0.017 Uiso 1 1 calc R . . . . C4 C 0.1389(2) 0.54391(14) 0.91361(17) 0.0177(5) Uani 1 1 d . . . . . H4 H 0.1316 0.4913 0.9478 0.021 Uiso 1 1 calc R . . . . C5 C 0.0279(2) 0.58467(15) 0.86618(17) 0.0178(5) Uani 1 1 d . . . . . H5 H -0.0549 0.5602 0.8690 0.021 Uiso 1 1 calc R . . . . C6 C 0.0373(2) 0.66094(15) 0.81480(17) 0.0170(5) Uani 1 1 d . . . . . H6 H -0.0389 0.6883 0.7818 0.020 Uiso 1 1 calc R . . . . C7 C 0.1579(2) 0.69734(14) 0.81159(17) 0.0145(5) Uani 1 1 d . . . . . H7 H 0.1646 0.7497 0.7766 0.017 Uiso 1 1 calc R . . . . C8 C 0.4728(2) 0.70044(13) 0.73025(16) 0.0118(4) Uani 1 1 d . . . . . C9 C 0.4269(2) 0.63304(13) 0.66573(16) 0.0129(4) Uani 1 1 d . . . . . H9 H 0.3673 0.5939 0.6884 0.015 Uiso 1 1 calc R . . . . C10 C 0.4693(2) 0.62357(14) 0.56805(17) 0.0149(5) Uani 1 1 d . . . . . H10 H 0.4388 0.5776 0.5239 0.018 Uiso 1 1 calc R . . . . C11 C 0.5556(2) 0.68073(15) 0.53456(18) 0.0183(5) Uani 1 1 d . . . . . H11 H 0.5826 0.6745 0.4670 0.022 Uiso 1 1 calc R . . . . C12 C 0.6026(2) 0.74721(15) 0.59952(19) 0.0201(5) Uani 1 1 d . . . . . H12 H 0.6628 0.7859 0.5767 0.024 Uiso 1 1 calc R . . . . C13 C 0.5620(2) 0.75727(15) 0.69765(18) 0.0167(5) Uani 1 1 d . . . . . H13 H 0.5945 0.8025 0.7424 0.020 Uiso 1 1 calc R . . . . C14 C 0.4027(2) 0.81617(13) 0.89643(17) 0.0118(4) Uani 1 1 d . . . . . C15 C 0.4017(2) 0.83293(14) 1.00348(17) 0.0151(5) Uani 1 1 d . . . . . H15 H 0.4207 0.7895 1.0545 0.018 Uiso 1 1 calc R . . . . C16 C 0.3727(2) 0.91387(14) 1.03435(18) 0.0179(5) Uani 1 1 d . . . . . H16 H 0.3721 0.9258 1.1070 0.021 Uiso 1 1 calc R . . . . C17 C 0.3449(2) 0.97708(15) 0.96082(19) 0.0191(5) Uani 1 1 d . . . . . H17 H 0.3246 1.0321 0.9830 0.023 Uiso 1 1 calc R . . . . C18 C 0.3463(2) 0.96046(15) 0.85445(18) 0.0191(5) Uani 1 1 d . . . . . H18 H 0.3278 1.0042 0.8039 0.023 Uiso 1 1 calc R . . . . C19 C 0.3748(2) 0.87973(14) 0.82181(18) 0.0166(5) Uani 1 1 d . . . . . H19 H 0.3752 0.8681 0.7490 0.020 Uiso 1 1 calc R . . . . S1A S 0.54205(5) 0.41699(3) 0.77880(4) 0.01335(12) Uani 1 1 d . . . . . F1A F 0.79206(13) 0.43901(9) 0.83720(11) 0.0239(3) Uani 1 1 d . . . . . F2A F 0.70110(14) 0.53789(8) 0.73785(11) 0.0260(3) Uani 1 1 d . . . . . F3A F 0.74012(14) 0.41722(9) 0.67046(11) 0.0271(3) Uani 1 1 d . . . . . O1A O 0.46298(16) 0.42673(11) 0.67876(13) 0.0229(4) Uani 1 1 d . . . . . O2A O 0.56769(16) 0.33097(9) 0.81350(13) 0.0194(4) Uani 1 1 d . . . . . O3A O 0.51213(16) 0.47303(10) 0.86115(12) 0.0203(4) Uani 1 1 d . . . . . C1A C 0.7012(2) 0.45460(14) 0.75423(17) 0.0159(5) Uani 1 1 d . . . . . 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 I1 0.01206(9) 0.02655(10) 0.02383(10) 0.00283(7) -0.00293(6) -0.00427(6) P1 0.0097(3) 0.0111(3) 0.0092(3) -0.0003(2) 0.0013(2) -0.0011(2) C1 0.0108(10) 0.0142(11) 0.0132(11) 0.0004(9) -0.0010(8) -0.0026(8) C2 0.0101(10) 0.0132(10) 0.0119(10) -0.0023(9) 0.0028(8) -0.0023(8) C3 0.0132(11) 0.0156(11) 0.0124(11) -0.0004(9) 0.0012(8) -0.0002(9) C4 0.0219(13) 0.0161(11) 0.0154(12) 0.0005(9) 0.0033(9) -0.0058(10) C5 0.0147(11) 0.0228(12) 0.0167(12) -0.0046(10) 0.0045(9) -0.0065(10) C6 0.0127(11) 0.0215(12) 0.0162(11) -0.0006(10) 0.0005(8) -0.0003(9) C7 0.0135(11) 0.0151(11) 0.0147(11) 0.0007(9) 0.0011(8) -0.0019(9) C8 0.0111(10) 0.0140(10) 0.0101(10) 0.0011(8) 0.0007(8) 0.0004(8) C9 0.0100(10) 0.0134(11) 0.0145(11) 0.0009(9) -0.0009(8) -0.0014(8) C10 0.0144(11) 0.0150(11) 0.0142(11) -0.0036(9) -0.0020(8) 0.0025(9) C11 0.0194(12) 0.0220(12) 0.0140(11) 0.0005(10) 0.0045(9) 0.0034(10) C12 0.0215(13) 0.0193(12) 0.0212(13) 0.0009(10) 0.0090(10) -0.0041(10) C13 0.0188(12) 0.0164(11) 0.0154(12) -0.0026(9) 0.0047(9) -0.0046(9) C14 0.0080(10) 0.0114(10) 0.0160(11) -0.0017(9) 0.0021(8) -0.0019(8) C15 0.0155(11) 0.0161(11) 0.0141(11) 0.0007(9) 0.0035(8) -0.0011(9) C16 0.0186(12) 0.0212(12) 0.0147(11) -0.0055(9) 0.0054(9) -0.0011(10) C17 0.0151(12) 0.0164(11) 0.0267(13) -0.0044(10) 0.0061(9) 0.0001(9) C18 0.0173(12) 0.0174(12) 0.0223(13) 0.0041(10) 0.0022(9) 0.0028(9) C19 0.0172(12) 0.0178(11) 0.0150(11) -0.0008(9) 0.0026(9) -0.0012(9) S1A 0.0149(3) 0.0122(3) 0.0133(3) -0.0013(2) 0.0030(2) -0.0020(2) F1A 0.0181(7) 0.0244(7) 0.0264(8) 0.0042(6) -0.0068(6) -0.0022(6) F2A 0.0230(8) 0.0167(7) 0.0388(9) 0.0109(6) 0.0056(6) -0.0029(6) F3A 0.0253(8) 0.0363(9) 0.0224(7) 0.0001(7) 0.0133(6) 0.0049(7) O1A 0.0201(9) 0.0263(9) 0.0206(9) -0.0022(7) -0.0035(7) -0.0015(7) O2A 0.0272(9) 0.0101(8) 0.0219(9) 0.0002(7) 0.0070(7) -0.0021(7) O3A 0.0268(9) 0.0168(8) 0.0193(9) -0.0033(7) 0.0100(7) 0.0005(7) C1A 0.0171(11) 0.0147(11) 0.0158(11) 0.0032(9) 0.0016(9) 0.0015(9) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' 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 C1 P1 C2 107.17(10) . . ? C8 P1 C1 110.35(10) . . ? C8 P1 C2 109.95(10) . . ? C8 P1 C14 111.96(10) . . ? C14 P1 C1 110.27(10) . . ? C14 P1 C2 106.96(10) . . ? P1 C1 I1 112.88(10) . . ? C3 C2 P1 121.68(17) . . ? C3 C2 C7 120.3(2) . . ? C7 C2 P1 117.93(16) . . ? C4 C3 C2 119.1(2) . . ? C5 C4 C3 120.6(2) . . ? C6 C5 C4 120.3(2) . . ? C5 C6 C7 120.0(2) . . ? C6 C7 C2 119.6(2) . . ? C9 C8 P1 118.74(16) . . ? C9 C8 C13 120.32(19) . . ? C13 C8 P1 120.81(16) . . ? C10 C9 C8 119.4(2) . . ? C11 C10 C9 120.5(2) . . ? C10 C11 C12 120.1(2) . . ? C13 C12 C11 120.2(2) . . ? C12 C13 C8 119.5(2) . . ? C15 C14 P1 117.45(16) . . ? C19 C14 P1 121.81(16) . . ? C19 C14 C15 120.4(2) . . ? C16 C15 C14 119.1(2) . . ? C17 C16 C15 120.8(2) . . ? C16 C17 C18 120.1(2) . . ? C17 C18 C19 120.0(2) . . ? C18 C19 C14 119.6(2) . . ? O1A S1A O2A 115.77(10) . . ? O1A S1A O3A 115.52(10) . . ? O1A S1A C1A 103.53(10) . . ? O2A S1A C1A 103.13(10) . . ? O3A S1A O2A 113.89(9) . . ? O3A S1A C1A 102.47(10) . . ? F1A C1A S1A 111.10(15) . . ? F2A C1A S1A 111.62(15) . . ? F2A C1A F1A 106.89(18) . . ? F3A C1A S1A 112.04(16) . . ? F3A C1A F1A 107.10(18) . . ? F3A C1A F2A 107.83(17) . . ? 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 I1 C1 2.139(2) . ? P1 C1 1.799(2) . ? P1 C2 1.802(2) . ? P1 C8 1.793(2) . ? P1 C14 1.795(2) . ? C2 C3 1.396(3) . ? C2 C7 1.403(3) . ? C3 C4 1.389(3) . ? C4 C5 1.388(3) . ? C5 C6 1.386(3) . ? C6 C7 1.387(3) . ? C8 C9 1.394(3) . ? C8 C13 1.398(3) . ? C9 C10 1.389(3) . ? C10 C11 1.384(3) . ? C11 C12 1.389(3) . ? C12 C13 1.388(3) . ? C14 C15 1.396(3) . ? C14 C19 1.391(3) . ? C15 C16 1.388(3) . ? C16 C17 1.378(3) . ? C17 C18 1.388(3) . ? C18 C19 1.391(3) . ? S1A O1A 1.4315(17) . ? S1A O2A 1.4477(16) . ? S1A O3A 1.4445(16) . ? S1A C1A 1.827(2) . ? F1A C1A 1.344(3) . ? F2A C1A 1.337(2) . ? F3A C1A 1.335(2) . ?