#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577311.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_1577311 loop_ _publ_author_name 'Fidelius, Jannis' 'Taube, Clemens' 'Schwedtmann, Kai' 'Hennersdorf, Felix' 'Gomila, Rosa Maria' 'Frontera, Antonio' 'Wolf, Robert' 'Weigand, Jan J.' _publ_section_title ; Imidazoliumyl-Substituted Di-and Iso-Tetraphosphanes and Their Metal-Mediated Fragmentation Reactions ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC02577C _journal_year 2026 _chemical_formula_moiety 'C17 H25 Cl N2 P, C6 H5 F, C F3 O3 S' _chemical_formula_sum 'C24 H30 Cl F4 N2 O3 P S' _chemical_formula_weight 568.98 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2026-01-11 _audit_creation_method ; Olex2 1.5 (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.6200(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.5631(2) _cell_length_b 9.37960(10) _cell_length_c 27.2987(4) _cell_measurement_reflns_used 6305 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 75.7820 _cell_measurement_theta_min 3.2590 _cell_volume 2686.66(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2850 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -56.00 34.00 0.50 3.00 -- -38.50 38.00 60.00 180 2 \w 25.00 71.00 0.50 3.00 -- 42.50-125.00-120.00 92 3 \w 25.00 56.00 0.50 3.00 -- 42.50-125.00-180.00 62 4 \w 77.00 102.00 0.50 12.00 -- 111.00 -94.00 -90.00 50 5 \w 76.00 121.00 0.50 12.00 -- 111.00-125.00 -60.00 90 6 \w 42.00 135.00 0.50 12.00 -- 111.00 -45.00-180.00 186 7 \w 118.00 175.00 0.50 12.00 -- 111.00 45.00 -60.00 114 8 \w 109.00 136.00 0.50 12.00 -- 111.00 125.00-120.00 54 9 \w 87.00 178.00 0.50 12.00 -- 111.00 30.00 0.00 182 10 \w 104.00 170.00 0.50 12.00 -- 111.00 45.00 30.00 132 11 \w 41.00 110.00 0.50 12.00 -- 111.00-125.00-180.00 138 12 \w 33.00 103.00 0.50 12.00 -- 111.00 -94.00-180.00 140 13 \w 34.00 59.00 0.50 12.00 -- 111.00 -94.00 60.00 50 14 \w 30.00 73.00 0.50 12.00 -- 111.00 -94.00 120.00 86 15 \w -92.00 -2.00 0.50 3.00 -- -38.50 125.00-120.00 180 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0680623000 _diffrn_orient_matrix_UB_12 -0.0031070000 _diffrn_orient_matrix_UB_13 0.0530453000 _diffrn_orient_matrix_UB_21 0.1071487000 _diffrn_orient_matrix_UB_22 0.0942852000 _diffrn_orient_matrix_UB_23 -0.0161155000 _diffrn_orient_matrix_UB_31 -0.0736993000 _diffrn_orient_matrix_UB_32 0.1344702000 _diffrn_orient_matrix_UB_33 0.0124749000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 14240 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.567 _diffrn_reflns_theta_min 3.260 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.055 _exptl_absorpt_correction_T_max 0.640 _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model 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 1.407 _exptl_crystal_description block _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.331 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.198 _refine_diff_density_max 0.553 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 5587 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0445 _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^)+(0.0687P)^2^+1.0264P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.1245 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4724 _reflns_number_total 5587 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1044 _cod_database_code 1577311 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C96 H100 Cl4 F16 N8 O12 P4 S4 ' _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. ; _reflns_odcompleteness_completeness 99.96 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)= Sof(H9AB)=Sof(H9AC)=1-FVAR(1) Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)= Sof(H9BB)=Sof(H9BC)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C4(H4), C7B(H7B), C7A(H7A) 3.b Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24) 3.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB, H9AC) ; _shelx_res_file ; TITL jjw1044_a.res in P2(1)/c jjw1044.res created by SHELXL-2018/3 at 20:18:06 on 11-Jan-2026 REM Old TITL jjw1044 in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.190, Rweak 0.048, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C24 N O4 F4 P Cl2 CELL 1.54184 10.5631 9.3796 27.2987 90 96.62 90 ZERR 4 0.0002 0.0001 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl F N O P S UNIT 96 120 4 16 8 12 4 4 L.S. 10 PLAN 5 TEMP 100 CONF BOND $H LIST 4 MORE -1 fmap 2 acta REM REM REM WGHT 0.068700 1.026400 FVAR 0.45652 0.51987 CL1 3 0.784902 0.351022 0.439313 11.00000 0.05859 0.05990 = 0.02449 0.01177 -0.00469 -0.02266 P1 7 0.675773 0.450540 0.381651 11.00000 0.02917 0.05819 = 0.02222 0.00067 0.00022 -0.02000 N1 5 0.811458 0.711961 0.409577 11.00000 0.01831 0.03659 = 0.02121 0.00166 0.00182 -0.00007 N2 5 0.606831 0.722449 0.411805 11.00000 0.01702 0.09387 = 0.02480 -0.01269 0.00096 -0.00004 C1 1 0.702105 0.635507 0.401181 11.00000 0.01955 0.06069 = 0.01991 -0.00422 0.00241 -0.00730 C2 1 0.784467 0.847047 0.425395 11.00000 0.02681 0.04156 = 0.02280 0.00271 0.00478 0.00648 C3 1 0.655187 0.853311 0.426705 11.00000 0.02854 0.06720 = 0.02218 -0.00108 0.00345 0.01377 C4 1 0.939949 0.654352 0.402722 11.00000 0.01727 0.03124 = 0.02465 -0.00272 0.00105 -0.00163 AFIX 13 H4 2 0.928091 0.553574 0.393887 11.00000 -1.20000 AFIX 0 C5 1 0.992977 0.726524 0.359683 11.00000 0.02474 0.04155 = 0.02617 -0.00094 0.00582 -0.00535 AFIX 137 H5A 2 0.931296 0.721621 0.331013 11.00000 -1.50000 H5B 2 1.069729 0.679056 0.353086 11.00000 -1.50000 H5C 2 1.011445 0.824538 0.367730 11.00000 -1.50000 AFIX 0 C6 1 1.029838 0.659003 0.450517 11.00000 0.02325 0.03836 = 0.02887 -0.00064 -0.00404 -0.00038 AFIX 137 H6A 2 1.056393 0.755545 0.457375 11.00000 -1.50000 H6B 2 1.103168 0.600865 0.447215 11.00000 -1.50000 H6C 2 0.986604 0.623531 0.477084 11.00000 -1.50000 AFIX 0 C10 1 0.878674 0.962036 0.439069 11.00000 0.04275 0.03365 = 0.04532 -0.00197 0.01216 0.00151 AFIX 137 H10A 2 0.926213 0.940005 0.470267 11.00000 -1.50000 H10B 2 0.834811 1.050952 0.441483 11.00000 -1.50000 H10C 2 0.935872 0.969456 0.414292 11.00000 -1.50000 AFIX 0 C11 1 0.580994 0.977238 0.442367 11.00000 0.04061 0.08897 = 0.03713 -0.00357 0.00735 0.03137 AFIX 137 H11A 2 0.520115 1.006802 0.415445 11.00000 -1.50000 H11B 2 0.638005 1.054647 0.451918 11.00000 -1.50000 H11C 2 0.537119 0.950016 0.469818 11.00000 -1.50000 AFIX 0 C12 1 0.776324 0.440003 0.331863 11.00000 0.02657 0.03472 = 0.02180 -0.00170 -0.00220 -0.01009 C13 1 0.870580 0.337455 0.329130 11.00000 0.03504 0.03179 = 0.03202 0.00466 -0.00557 -0.00471 AFIX 43 H13 2 0.892055 0.275602 0.355402 11.00000 -1.20000 AFIX 0 C14 1 0.932038 0.327956 0.287262 11.00000 0.03513 0.03419 = 0.04021 -0.00330 0.00103 0.00292 AFIX 43 H14 2 0.995535 0.260032 0.285592 11.00000 -1.20000 AFIX 0 C15 1 0.899940 0.418812 0.247657 11.00000 0.03681 0.03818 = 0.02787 -0.00619 0.00708 -0.00171 AFIX 43 H15 2 0.941141 0.410805 0.219457 11.00000 -1.20000 AFIX 0 C16 1 0.806500 0.521501 0.250102 11.00000 0.03155 0.03577 = 0.02139 -0.00132 -0.00081 -0.00402 AFIX 43 H16 2 0.785395 0.583038 0.223710 11.00000 -1.20000 AFIX 0 C17 1 0.744673 0.532032 0.292065 11.00000 0.02412 0.03620 = 0.02283 -0.00127 -0.00090 -0.00047 AFIX 43 H17 2 0.681803 0.600689 0.293749 11.00000 -1.20000 AFIX 0 PART 1 C7B 1 0.465369 0.720547 0.407263 21.00000 0.01434 0.04149 = 0.03758 0.00126 0.00292 0.00008 AFIX 13 H7B 2 0.434193 0.817858 0.411091 21.00000 -1.20000 AFIX 0 C8B 1 0.436048 0.633767 0.449559 21.00000 0.02678 0.09165 = 0.03342 -0.00335 0.01144 -0.02181 AFIX 137 H8BA 2 0.472821 0.540669 0.447500 21.00000 -1.50000 H8BB 2 0.345330 0.625251 0.449019 21.00000 -1.50000 H8BC 2 0.470901 0.678880 0.479696 21.00000 -1.50000 AFIX 0 C9B 1 0.407024 0.661448 0.357864 21.00000 0.02397 0.03828 = 0.03530 -0.00252 -0.00337 -0.00214 AFIX 137 H9BA 2 0.443985 0.708586 0.331718 21.00000 -1.50000 H9BB 2 0.316666 0.677495 0.354126 21.00000 -1.50000 H9BC 2 0.423600 0.560965 0.356573 21.00000 -1.50000 AFIX 0 PART 2 C7A 1 0.472339 0.641610 0.412751 -21.00000 0.01585 0.03002 = 0.03958 0.00371 0.00808 0.00119 AFIX 13 H7A 2 0.485627 0.539076 0.408704 -21.00000 -1.20000 AFIX 0 C8A 1 0.417203 0.666292 0.461043 -21.00000 0.02916 0.06032 = 0.03116 0.00305 0.01750 -0.00295 AFIX 137 H8AA 2 0.346676 0.602857 0.463073 -21.00000 -1.50000 H8AB 2 0.388480 0.763154 0.462444 -21.00000 -1.50000 H8AC 2 0.481609 0.648463 0.488130 -21.00000 -1.50000 AFIX 0 C9A 1 0.389415 0.697114 0.367622 -21.00000 0.02555 0.04029 = 0.04057 -0.00698 -0.00136 -0.00509 AFIX 137 H9AA 2 0.377622 0.798036 0.370802 -21.00000 -1.50000 H9AB 2 0.308072 0.650336 0.364905 -21.00000 -1.50000 H9AC 2 0.430142 0.678050 0.338637 -21.00000 -1.50000 AFIX 0 PART 0 F4 4 0.329254 0.600980 0.159734 11.00000 0.05667 0.04251 = 0.04721 0.00985 0.00767 0.01248 C19 1 0.348175 0.512161 0.199312 11.00000 0.04293 0.02937 = 0.03623 -0.00044 0.00409 -0.00138 C20 1 0.250039 0.490348 0.227605 11.00000 0.04138 0.03975 = 0.06568 0.00066 0.01470 -0.00005 AFIX 43 H20 2 0.171101 0.533475 0.219559 11.00000 -1.20000 AFIX 0 C21 1 0.272638 0.401659 0.268667 11.00000 0.05649 0.04597 = 0.05718 -0.00155 0.02281 -0.01439 AFIX 43 H21 2 0.208771 0.387173 0.288909 11.00000 -1.20000 AFIX 0 C22 1 0.389194 0.335128 0.279516 11.00000 0.05822 0.03808 = 0.03670 0.00167 0.00058 -0.01891 AFIX 43 H22 2 0.403197 0.274655 0.306597 11.00000 -1.20000 AFIX 0 C23 1 0.484774 0.358774 0.250001 11.00000 0.03775 0.03624 = 0.04306 0.00278 -0.00722 -0.01067 AFIX 43 H23 2 0.562940 0.313348 0.257274 11.00000 -1.20000 AFIX 0 C24 1 0.465884 0.449395 0.209614 11.00000 0.03414 0.03643 = 0.03906 -0.00037 0.00356 -0.00674 AFIX 43 H24 2 0.530810 0.467104 0.190132 11.00000 -1.20000 AFIX 0 S1 8 0.214463 0.081357 0.394560 11.00000 0.02582 0.03444 = 0.02371 0.00320 0.00141 -0.00114 F1 4 0.215806 0.361541 0.392681 11.00000 0.10251 0.03717 = 0.04776 0.00077 0.00478 -0.01248 F2 4 0.122563 0.270323 0.451202 11.00000 0.12072 0.06774 = 0.05910 -0.01680 0.04564 0.00844 F3 4 0.326813 0.268746 0.455792 11.00000 0.11168 0.07937 = 0.05138 -0.00588 -0.02815 -0.04110 O1 6 0.324273 0.083759 0.368078 11.00000 0.03072 0.06415 = 0.03359 0.00757 0.00842 0.00518 O2 6 0.094414 0.086137 0.363668 11.00000 0.02927 0.04203 = 0.03495 0.00214 -0.00349 -0.00210 O3 6 0.220884 -0.017237 0.435186 11.00000 0.04505 0.04777 = 0.03564 0.01417 0.00129 -0.00118 C18 1 0.220442 0.254011 0.425095 11.00000 0.06559 0.04450 = 0.02814 -0.00484 0.00372 -0.01121 HKLF 4 REM jjw1044_a.res in P2(1)/c REM wR2 = 0.1245, GooF = S = 1.021, Restrained GooF = 1.021 for all data REM R1 = 0.0445 for 4724 Fo > 4sig(Fo) and 0.0532 for all 5587 data REM 361 parameters refined using 0 restraints END WGHT 0.0687 1.0264 REM Highest difference peak 0.553, deepest hole -0.703, 1-sigma level 0.058 Q1 1 0.7443 0.4022 0.4100 11.00000 0.05 0.55 Q2 1 0.7500 0.4519 0.3568 11.00000 0.05 0.40 Q3 1 0.7122 0.4435 0.3523 11.00000 0.05 0.38 Q4 1 0.2294 0.0643 0.4284 11.00000 0.05 0.37 Q5 1 0.2306 0.1422 0.4213 11.00000 0.05 0.32 ; _shelx_res_checksum 39738 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.035 _oxdiff_exptl_absorpt_empirical_full_min 0.760 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_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 Cl1 Cl 0.78490(6) 0.35102(7) 0.43931(2) 0.04840(17) Uani 1 1 d . . . . . P1 P 0.67577(5) 0.45054(7) 0.38165(2) 0.03674(15) Uani 1 1 d . . . . . N1 N 0.81146(14) 0.71196(18) 0.40958(6) 0.0254(3) Uani 1 1 d . . . . . N2 N 0.60683(16) 0.7224(3) 0.41180(7) 0.0453(5) Uani 1 1 d . . . . . C1 C 0.70210(18) 0.6355(3) 0.40118(7) 0.0334(4) Uani 1 1 d . . . . . C2 C 0.78447(18) 0.8470(2) 0.42540(7) 0.0302(4) Uani 1 1 d . . . . . C3 C 0.6552(2) 0.8533(3) 0.42670(8) 0.0393(5) Uani 1 1 d . . . . . C4 C 0.93995(16) 0.6544(2) 0.40272(7) 0.0245(4) Uani 1 1 d . . . . . H4 H 0.928091 0.553574 0.393887 0.029 Uiso 1 1 calc R U . . . C5 C 0.99298(18) 0.7265(2) 0.35968(7) 0.0306(4) Uani 1 1 d . . . . . H5A H 0.931296 0.721621 0.331013 0.046 Uiso 1 1 calc R U . . . H5B H 1.069729 0.679056 0.353086 0.046 Uiso 1 1 calc R U . . . H5C H 1.011445 0.824538 0.367730 0.046 Uiso 1 1 calc R U . . . C6 C 1.02984(18) 0.6590(2) 0.45052(7) 0.0307(4) Uani 1 1 d . . . . . H6A H 1.056393 0.755545 0.457375 0.046 Uiso 1 1 calc R U . . . H6B H 1.103168 0.600865 0.447215 0.046 Uiso 1 1 calc R U . . . H6C H 0.986604 0.623531 0.477084 0.046 Uiso 1 1 calc R U . . . C10 C 0.8787(2) 0.9620(2) 0.43907(9) 0.0400(5) Uani 1 1 d . . . . . H10A H 0.926213 0.940005 0.470267 0.060 Uiso 1 1 calc R U . . . H10B H 0.834811 1.050952 0.441483 0.060 Uiso 1 1 calc R U . . . H10C H 0.935872 0.969456 0.414292 0.060 Uiso 1 1 calc R U . . . C11 C 0.5810(2) 0.9772(4) 0.44237(10) 0.0553(7) Uani 1 1 d . . . . . H11A H 0.520115 1.006802 0.415445 0.083 Uiso 1 1 calc R U . . . H11B H 0.638005 1.054647 0.451918 0.083 Uiso 1 1 calc R U . . . H11C H 0.537119 0.950016 0.469818 0.083 Uiso 1 1 calc R U . . . C12 C 0.77632(18) 0.4400(2) 0.33186(7) 0.0281(4) Uani 1 1 d . . . . . C13 C 0.8706(2) 0.3375(2) 0.32913(8) 0.0337(4) Uani 1 1 d . . . . . H13 H 0.892055 0.275602 0.355402 0.040 Uiso 1 1 calc R U . . . C14 C 0.9320(2) 0.3280(2) 0.28726(9) 0.0368(5) Uani 1 1 d . . . . . H14 H 0.995535 0.260032 0.285592 0.044 Uiso 1 1 calc R U . . . C15 C 0.8999(2) 0.4188(2) 0.24766(8) 0.0340(4) Uani 1 1 d . . . . . H15 H 0.941141 0.410805 0.219457 0.041 Uiso 1 1 calc R U . . . C16 C 0.80650(19) 0.5215(2) 0.25010(7) 0.0299(4) Uani 1 1 d . . . . . H16 H 0.785395 0.583038 0.223710 0.036 Uiso 1 1 calc R U . . . C17 C 0.74467(17) 0.5320(2) 0.29206(7) 0.0280(4) Uani 1 1 d . . . . . H17 H 0.681803 0.600689 0.293749 0.034 Uiso 1 1 calc R U . . . C7B C 0.4654(3) 0.7205(10) 0.40726(17) 0.0311(15) Uani 0.520(13) 1 d . . P A 1 H7B H 0.434193 0.817858 0.411091 0.037 Uiso 0.520(13) 1 calc R U P A 1 C8B C 0.4360(10) 0.6338(15) 0.4496(4) 0.050(2) Uani 0.520(13) 1 d . . P A 1 H8BA H 0.472821 0.540669 0.447500 0.075 Uiso 0.520(13) 1 calc R U P A 1 H8BB H 0.345330 0.625251 0.449019 0.075 Uiso 0.520(13) 1 calc R U P A 1 H8BC H 0.470901 0.678880 0.479696 0.075 Uiso 0.520(13) 1 calc R U P A 1 C9B C 0.4070(10) 0.6614(11) 0.3579(4) 0.0330(17) Uani 0.520(13) 1 d . . P A 1 H9BA H 0.443985 0.708586 0.331718 0.050 Uiso 0.520(13) 1 calc R U P A 1 H9BB H 0.316666 0.677495 0.354126 0.050 Uiso 0.520(13) 1 calc R U P A 1 H9BC H 0.423600 0.560965 0.356573 0.050 Uiso 0.520(13) 1 calc R U P A 1 C7A C 0.4723(4) 0.6416(10) 0.41275(18) 0.0281(15) Uani 0.480(13) 1 d . . P A 2 H7A H 0.485627 0.539076 0.408704 0.034 Uiso 0.480(13) 1 calc R U P A 2 C8A C 0.4172(10) 0.6663(13) 0.4610(4) 0.0391(19) Uani 0.480(13) 1 d . . P A 2 H8AA H 0.346676 0.602857 0.463073 0.059 Uiso 0.480(13) 1 calc R U P A 2 H8AB H 0.388480 0.763154 0.462444 0.059 Uiso 0.480(13) 1 calc R U P A 2 H8AC H 0.481609 0.648463 0.488130 0.059 Uiso 0.480(13) 1 calc R U P A 2 C9A C 0.3894(11) 0.6971(12) 0.3676(4) 0.036(2) Uani 0.480(13) 1 d . . P A 2 H9AA H 0.377622 0.798036 0.370802 0.054 Uiso 0.480(13) 1 calc R U P A 2 H9AB H 0.308072 0.650336 0.364905 0.054 Uiso 0.480(13) 1 calc R U P A 2 H9AC H 0.430142 0.678050 0.338637 0.054 Uiso 0.480(13) 1 calc R U P A 2 F4 F 0.32925(15) 0.60098(16) 0.15973(6) 0.0487(3) Uani 1 1 d . . . . . C19 C 0.3482(2) 0.5122(2) 0.19931(8) 0.0362(4) Uani 1 1 d . . . . . C20 C 0.2500(2) 0.4903(3) 0.22760(11) 0.0483(6) Uani 1 1 d . . . . . H20 H 0.171101 0.533475 0.219559 0.058 Uiso 1 1 calc R U . . . C21 C 0.2726(3) 0.4017(3) 0.26867(11) 0.0519(6) Uani 1 1 d . . . . . H21 H 0.208771 0.387173 0.288909 0.062 Uiso 1 1 calc R U . . . C22 C 0.3892(3) 0.3351(3) 0.27952(9) 0.0447(6) Uani 1 1 d . . . . . H22 H 0.403197 0.274655 0.306597 0.054 Uiso 1 1 calc R U . . . C23 C 0.4848(2) 0.3588(2) 0.25000(9) 0.0399(5) Uani 1 1 d . . . . . H23 H 0.562940 0.313348 0.257274 0.048 Uiso 1 1 calc R U . . . C24 C 0.4659(2) 0.4494(2) 0.20961(9) 0.0366(5) Uani 1 1 d . . . . . H24 H 0.530810 0.467104 0.190132 0.044 Uiso 1 1 calc R U . . . S1 S 0.21446(4) 0.08136(5) 0.39456(2) 0.02810(13) Uani 1 1 d . . . . . F1 F 0.2158(2) 0.36154(16) 0.39268(6) 0.0628(5) Uani 1 1 d . . . . . F2 F 0.1226(2) 0.2703(2) 0.45120(7) 0.0798(6) Uani 1 1 d . . . . . F3 F 0.3268(2) 0.2687(2) 0.45579(7) 0.0837(7) Uani 1 1 d . . . . . O1 O 0.32427(15) 0.0838(2) 0.36808(6) 0.0425(4) Uani 1 1 d . . . . . O2 O 0.09441(14) 0.08614(17) 0.36367(6) 0.0360(3) Uani 1 1 d . . . . . O3 O 0.22088(16) -0.01724(19) 0.43519(6) 0.0431(4) Uani 1 1 d . . . . . C18 C 0.2204(3) 0.2540(3) 0.42509(9) 0.0462(6) 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 Cl1 0.0586(3) 0.0599(4) 0.0245(2) 0.0118(2) -0.0047(2) -0.0227(3) P1 0.0292(3) 0.0582(3) 0.0222(2) 0.0007(2) 0.00022(18) -0.0200(2) N1 0.0183(7) 0.0366(8) 0.0212(7) 0.0017(6) 0.0018(5) -0.0001(6) N2 0.0170(7) 0.0939(17) 0.0248(8) -0.0127(10) 0.0010(6) 0.0000(9) C1 0.0195(8) 0.0607(13) 0.0199(8) -0.0042(8) 0.0024(7) -0.0073(8) C2 0.0268(9) 0.0416(11) 0.0228(9) 0.0027(8) 0.0048(7) 0.0065(8) C3 0.0285(10) 0.0672(15) 0.0222(9) -0.0011(9) 0.0034(7) 0.0138(10) C4 0.0173(7) 0.0312(9) 0.0247(9) -0.0027(7) 0.0011(6) -0.0016(6) C5 0.0247(8) 0.0416(11) 0.0262(9) -0.0009(8) 0.0058(7) -0.0053(8) C6 0.0233(8) 0.0384(10) 0.0289(9) -0.0006(8) -0.0040(7) -0.0004(7) C10 0.0427(11) 0.0337(11) 0.0453(13) -0.0020(9) 0.0122(10) 0.0015(9) C11 0.0406(12) 0.089(2) 0.0371(12) -0.0036(13) 0.0074(10) 0.0314(13) C12 0.0266(8) 0.0347(10) 0.0218(8) -0.0017(7) -0.0022(7) -0.0101(7) C13 0.0350(10) 0.0318(10) 0.0320(10) 0.0047(8) -0.0056(8) -0.0047(8) C14 0.0351(10) 0.0342(10) 0.0402(12) -0.0033(9) 0.0010(8) 0.0029(8) C15 0.0368(10) 0.0382(11) 0.0279(10) -0.0062(8) 0.0071(8) -0.0017(8) C16 0.0315(9) 0.0358(10) 0.0214(9) -0.0013(7) -0.0008(7) -0.0040(8) C17 0.0241(8) 0.0362(10) 0.0228(9) -0.0013(7) -0.0009(7) -0.0005(7) C7B 0.0143(17) 0.041(4) 0.038(2) 0.001(2) 0.0029(14) 0.0001(18) C8B 0.027(4) 0.092(7) 0.033(5) -0.003(4) 0.011(3) -0.022(4) C9B 0.024(3) 0.038(4) 0.035(4) -0.003(3) -0.003(2) -0.002(3) C7A 0.0158(18) 0.030(4) 0.040(3) 0.004(2) 0.0081(16) 0.0012(18) C8A 0.029(3) 0.060(5) 0.031(5) 0.003(3) 0.018(3) -0.003(3) C9A 0.026(4) 0.040(5) 0.041(5) -0.007(3) -0.001(3) -0.005(3) F4 0.0567(8) 0.0425(7) 0.0472(8) 0.0099(6) 0.0077(6) 0.0125(6) C19 0.0429(11) 0.0294(10) 0.0362(11) -0.0004(8) 0.0041(9) -0.0014(8) C20 0.0414(12) 0.0398(12) 0.0657(17) 0.0007(11) 0.0147(11) 0.0000(10) C21 0.0565(15) 0.0460(13) 0.0572(16) -0.0015(12) 0.0228(12) -0.0144(11) C22 0.0582(14) 0.0381(12) 0.0367(12) 0.0017(9) 0.0006(10) -0.0189(10) C23 0.0377(11) 0.0362(11) 0.0431(12) 0.0028(9) -0.0072(9) -0.0107(9) C24 0.0341(10) 0.0364(11) 0.0391(11) -0.0004(9) 0.0036(9) -0.0067(8) S1 0.0258(2) 0.0344(2) 0.0237(2) 0.00320(17) 0.00141(17) -0.00114(17) F1 0.1025(14) 0.0372(8) 0.0478(9) 0.0008(6) 0.0048(9) -0.0125(8) F2 0.1207(17) 0.0677(11) 0.0591(11) -0.0168(9) 0.0456(11) 0.0084(11) F3 0.1117(16) 0.0794(13) 0.0514(10) -0.0059(9) -0.0281(10) -0.0411(12) O1 0.0307(7) 0.0641(11) 0.0336(8) 0.0076(7) 0.0084(6) 0.0052(7) O2 0.0293(7) 0.0420(8) 0.0349(8) 0.0021(6) -0.0035(6) -0.0021(6) O3 0.0450(9) 0.0478(9) 0.0356(8) 0.0142(7) 0.0013(7) -0.0012(7) C18 0.0656(16) 0.0445(13) 0.0281(11) -0.0048(9) 0.0037(10) -0.0112(11) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 3 1 -5 0.0953 1 0 -5 0.1001 1 1 -5 0.0975 -1 1 5 0.1262 -1 1 -5 0.1050 0 0 -1 0.0787 0 0 1 0.1194 4 -3 -5 0.1486 -3 1 5 0.1291 3 4 -5 0.1247 0 -1 5 0.1511 5 2 0 0.1123 5 0 -2 0.1271 4 5 3 0.1289 -2 -2 -5 0.1070 -5 1 -4 0.1004 -4 5 5 0.1548 5 -1 5 0.1378 1 -1 5 0.1508 -5 -3 -1 0.1084 1 2 5 0.1300 -3 -1 -5 0.0813 3 1 5 0.1266 -3 -4 5 0.1328 -1 5 1 0.1504 2 -5 -2 0.1634 -3 -1 5 0.1090 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 Cl1 98.86(7) . . ? C12 P1 Cl1 102.83(7) . . ? C12 P1 C1 100.78(9) . . ? C1 N1 C2 109.63(17) . . ? C1 N1 C4 123.81(17) . . ? C2 N1 C4 126.57(16) . . ? C1 N2 C3 110.00(17) . . ? C1 N2 C7B 137.8(4) . . ? C1 N2 C7A 113.5(4) . . ? C3 N2 C7B 111.8(4) . . ? C3 N2 C7A 135.5(3) . . ? N1 C1 P1 130.50(16) . . ? N2 C1 P1 122.90(16) . . ? N2 C1 N1 106.6(2) . . ? N1 C2 C10 126.09(18) . . ? C3 C2 N1 106.86(19) . . ? C3 C2 C10 127.0(2) . . ? N2 C3 C11 126.3(2) . . ? C2 C3 N2 106.9(2) . . ? C2 C3 C11 126.8(3) . . ? N1 C4 H4 106.7 . . ? N1 C4 C5 110.96(15) . . ? N1 C4 C6 111.61(15) . . ? C5 C4 H4 106.7 . . ? C5 C4 C6 113.64(15) . . ? C6 C4 H4 106.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P1 124.02(16) . . ? C13 C12 C17 119.56(19) . . ? C17 C12 P1 116.02(15) . . ? C12 C13 H13 120.1 . . ? C14 C13 C12 119.75(19) . . ? C14 C13 H13 120.1 . . ? C13 C14 H14 119.7 . . ? C13 C14 C15 120.6(2) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 120.0 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C15 C16 H16 120.2 . . ? C17 C16 C15 119.69(19) . . ? C17 C16 H16 120.2 . . ? C12 C17 H17 119.8 . . ? C16 C17 C12 120.34(19) . . ? C16 C17 H17 119.8 . . ? N2 C7B H7B 109.1 . . ? N2 C7B C9B 112.3(5) . . ? C8B C7B N2 104.0(7) . . ? C8B C7B H7B 109.1 . . ? C8B C7B C9B 113.1(9) . . ? C9B C7B H7B 109.1 . . ? C7B C8B H8BA 109.5 . . ? C7B C8B H8BB 109.5 . . ? C7B C8B H8BC 109.5 . . ? H8BA C8B H8BB 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? C7B C9B H9BA 109.5 . . ? C7B C9B H9BB 109.5 . . ? C7B C9B H9BC 109.5 . . ? H9BA C9B H9BB 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? N2 C7A H7A 108.8 . . ? C8A C7A N2 111.6(6) . . ? C8A C7A H7A 108.8 . . ? C9A C7A N2 104.6(6) . . ? C9A C7A H7A 108.8 . . ? C9A C7A C8A 114.1(8) . . ? C7A C8A H8AA 109.5 . . ? C7A C8A H8AB 109.5 . . ? C7A C8A H8AC 109.5 . . ? H8AA C8A H8AB 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C7A C9A H9AA 109.5 . . ? C7A C9A H9AB 109.5 . . ? C7A C9A H9AC 109.5 . . ? H9AA C9A H9AB 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? F4 C19 C20 119.0(2) . . ? F4 C19 C24 118.1(2) . . ? C24 C19 C20 122.9(2) . . ? C19 C20 H20 121.0 . . ? C19 C20 C21 118.0(2) . . ? C21 C20 H20 121.0 . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21 119.7 . . ? C21 C22 H22 120.1 . . ? C23 C22 C21 119.7(2) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 119.5 . . ? C22 C23 C24 120.9(2) . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 117.9(2) . . ? C19 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? O1 S1 O2 114.36(10) . . ? O1 S1 O3 115.40(10) . . ? O1 S1 C18 103.26(12) . . ? O2 S1 C18 102.84(11) . . ? O3 S1 O2 115.54(10) . . ? O3 S1 C18 102.87(11) . . ? F1 C18 S1 111.78(16) . . ? F2 C18 S1 111.09(19) . . ? F2 C18 F1 107.2(2) . . ? F3 C18 S1 111.3(2) . . ? F3 C18 F1 107.6(2) . . ? F3 C18 F2 107.6(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 Cl1 P1 2.0639(8) . ? P1 C1 1.827(2) . ? P1 C12 1.822(2) . ? N1 C1 1.356(2) . ? N1 C2 1.379(3) . ? N1 C4 1.493(2) . ? N2 C1 1.352(3) . ? N2 C3 1.373(4) . ? N2 C7B 1.485(4) . ? N2 C7A 1.613(5) . ? C2 C3 1.371(3) . ? C2 C10 1.486(3) . ? C3 C11 1.492(3) . ? C4 H4 0.9800 . ? C4 C5 1.518(3) . ? C4 C6 1.523(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.393(3) . ? C12 C17 1.398(3) . ? C13 H13 0.9300 . ? C13 C14 1.381(3) . ? C14 H14 0.9300 . ? C14 C15 1.388(3) . ? C15 H15 0.9300 . ? C15 C16 1.386(3) . ? C16 H16 0.9300 . ? C16 C17 1.386(3) . ? C17 H17 0.9300 . ? C7B H7B 0.9800 . ? C7B C8B 1.474(14) . ? C7B C9B 1.521(12) . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C9B H9BA 0.9600 . ? C9B H9BB 0.9600 . ? C9B H9BC 0.9600 . ? C7A H7A 0.9800 . ? C7A C8A 1.519(10) . ? C7A C9A 1.519(15) . ? C8A H8AA 0.9600 . ? C8A H8AB 0.9600 . ? C8A H8AC 0.9600 . ? C9A H9AA 0.9600 . ? C9A H9AB 0.9600 . ? C9A H9AC 0.9600 . ? F4 C19 1.361(3) . ? C19 C20 1.378(3) . ? C19 C24 1.375(3) . ? C20 H20 0.9300 . ? C20 C21 1.394(4) . ? C21 H21 0.9300 . ? C21 C22 1.382(4) . ? C22 H22 0.9300 . ? C22 C23 1.380(4) . ? C23 H23 0.9300 . ? C23 C24 1.388(3) . ? C24 H24 0.9300 . ? S1 O1 1.4359(16) . ? S1 O2 1.4404(14) . ? S1 O3 1.4396(16) . ? S1 C18 1.819(3) . ? F1 C18 1.339(3) . ? F2 C18 1.330(3) . ? F3 C18 1.329(3) . ? 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 Cl1 P1 C1 N1 59.65(19) . . . . ? Cl1 P1 C1 N2 -118.00(17) . . . . ? Cl1 P1 C12 C13 24.45(17) . . . . ? Cl1 P1 C12 C17 -162.86(13) . . . . ? P1 C12 C13 C14 172.65(16) . . . . ? P1 C12 C17 C16 -173.02(15) . . . . ? N1 C2 C3 N2 0.1(2) . . . . ? N1 C2 C3 C11 178.9(2) . . . . ? C1 P1 C12 C13 126.23(17) . . . . ? C1 P1 C12 C17 -61.07(16) . . . . ? C1 N1 C2 C3 0.0(2) . . . . ? C1 N1 C2 C10 179.1(2) . . . . ? C1 N1 C4 C5 111.9(2) . . . . ? C1 N1 C4 C6 -120.28(19) . . . . ? C1 N2 C3 C2 -0.2(2) . . . . ? C1 N2 C3 C11 -178.9(2) . . . . ? C1 N2 C7B C8B 79.8(7) . . . . ? C1 N2 C7B C9B -42.8(10) . . . . ? C1 N2 C7A C8A 125.9(7) . . . . ? C1 N2 C7A C9A -110.2(7) . . . . ? C2 N1 C1 P1 -178.04(16) . . . . ? C2 N1 C1 N2 -0.1(2) . . . . ? C2 N1 C4 C5 -68.7(2) . . . . ? C2 N1 C4 C6 59.1(2) . . . . ? C3 N2 C1 P1 178.30(15) . . . . ? C3 N2 C1 N1 0.2(2) . . . . ? C3 N2 C7B C8B -107.9(8) . . . . ? C3 N2 C7B C9B 129.5(7) . . . . ? C3 N2 C7A C8A -41.2(9) . . . . ? C3 N2 C7A C9A 82.7(6) . . . . ? C4 N1 C1 P1 1.5(3) . . . . ? C4 N1 C1 N2 179.40(16) . . . . ? C4 N1 C2 C3 -179.49(17) . . . . ? C4 N1 C2 C10 -0.4(3) . . . . ? C10 C2 C3 N2 -179.0(2) . . . . ? C10 C2 C3 C11 -0.2(4) . . . . ? C12 P1 C1 N1 -45.3(2) . . . . ? C12 P1 C1 N2 137.02(18) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C12 C17 C16 0.0(3) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C12 0.2(3) . . . . ? C17 C12 C13 C14 0.2(3) . . . . ? C7B N2 C1 P1 -9.3(5) . . . . ? C7B N2 C1 N1 172.6(4) . . . . ? C7B N2 C3 C2 -174.7(3) . . . . ? C7B N2 C3 C11 6.5(4) . . . . ? C7A N2 C1 P1 7.8(3) . . . . ? C7A N2 C1 N1 -170.3(3) . . . . ? C7A N2 C3 C2 167.3(4) . . . . ? C7A N2 C3 C11 -11.5(5) . . . . ? F4 C19 C20 C21 -178.5(2) . . . . ? F4 C19 C24 C23 -180.0(2) . . . . ? C19 C20 C21 C22 -1.7(4) . . . . ? C20 C19 C24 C23 0.9(3) . . . . ? C20 C21 C22 C23 1.2(4) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C22 C23 C24 C19 -1.5(3) . . . . ? C24 C19 C20 C21 0.7(4) . . . . ? O1 S1 C18 F1 59.4(2) . . . . ? O1 S1 C18 F2 179.15(19) . . . . ? O1 S1 C18 F3 -60.9(2) . . . . ? O2 S1 C18 F1 -59.8(2) . . . . ? O2 S1 C18 F2 59.9(2) . . . . ? O2 S1 C18 F3 179.86(18) . . . . ? O3 S1 C18 F1 179.8(2) . . . . ? O3 S1 C18 F2 -60.5(2) . . . . ? O3 S1 C18 F3 59.5(2) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 3.0000 1.0000 -5.0000 -0.0641 0.4963 -0.1490 1.0000 -0.0000 -5.0000 -0.1972 0.1877 -0.1361 1.0000 1.0000 -5.0000 -0.2003 0.2820 -0.0016 -1.0000 1.0000 5.0000 0.1941 -0.0934 0.2705 -1.0000 1.0000 -5.0000 -0.3364 0.0677 0.1458 -0.0000 -0.0000 -1.0000 -0.0530 0.0161 -0.0125 0.0000 0.0000 1.0000 0.0530 -0.0161 0.0125 4.0000 -3.0000 -5.0000 0.0163 0.2263 -0.7606 -3.0000 1.0000 5.0000 0.0579 -0.3077 0.4179 3.0000 4.0000 -5.0000 -0.0735 0.7792 0.2544 -0.0000 -1.0000 5.0000 0.2683 -0.1749 -0.0721 5.0000 2.0000 -0.0000 0.3341 0.7243 -0.0996 5.0000 0.0000 -2.0000 0.2342 0.5680 -0.3934 4.0000 5.0000 3.0000 0.4159 0.8517 0.4150 -2.0000 -2.0000 -5.0000 -0.3951 -0.3223 -0.1839 -5.0000 1.0000 -3.9999 -0.5556 -0.3770 0.4531 -4.0000 5.0000 5.0001 -0.0226 -0.0377 1.0295 5.0000 -1.0000 4.9999 0.6086 0.3609 -0.4406 1.0000 -1.0000 5.0000 0.3364 -0.0677 -0.1458 -5.0000 -3.0000 -1.0000 -0.3840 -0.8025 -0.0474 1.0000 2.0000 5.0000 0.3271 0.2151 0.2576 -3.0000 -1.0000 -5.0000 -0.4663 -0.3352 0.0243 3.0000 1.0000 5.0000 0.4663 0.3352 -0.0243 -3.0000 -4.0000 5.0000 0.0735 -0.7792 -0.2544 -1.0000 5.0000 1.0001 -0.0305 0.3482 0.7585 2.0000 -5.0000 -2.0001 0.0456 -0.2249 -0.8447 -3.0000 -1.0000 5.0000 0.0641 -0.4963 0.1490