#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577306.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_1577306 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_absolute_configuration ad _chemical_formula_moiety 'C51 H93 N6 P4, 3(C F3 O3 S), 3(C2 H3 N)' _chemical_formula_sum 'C60 H102 F9 N9 O9 P4 S3' _chemical_formula_weight 1484.56 _space_group_crystal_system trigonal _space_group_IT_number 161 _space_group_name_Hall 'R 3 -2"c' _space_group_name_H-M_alt 'R 3 c :H' _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 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 14.02799(8) _cell_length_b 14.02799(8) _cell_length_c 68.3806(5) _cell_measurement_reflns_used 21075 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 75.8460 _cell_measurement_theta_min 3.8380 _cell_volume 11653.45(13) _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 0.999 _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 -55.00 32.00 0.50 1.00 -- -41.74 38.00 -90.00 174 2 \w 6.00 49.00 0.50 1.00 -- 41.74 -99.00-180.00 86 3 \w 47.00 89.00 0.50 1.00 -- 41.74-125.00 -60.00 84 4 \w 73.00 116.00 0.50 4.00 -- 111.00-111.00 30.00 86 5 \w 65.00 107.00 0.50 4.00 -- 111.00 -94.00 60.00 84 6 \w 61.00 90.00 0.50 4.00 -- 111.00 -94.00 -30.00 58 7 \w 67.00 114.00 0.50 4.00 -- 111.00-111.00 -60.00 94 8 \w 51.00 121.00 0.50 4.00 -- 111.00 -61.00 30.00 140 9 \w 62.00 158.00 0.50 4.00 -- 111.00 15.00 30.00 192 10 \w 153.00 178.00 0.50 4.00 -- 111.00 45.00 -60.00 50 11 \w 134.00 168.00 0.50 4.00 -- 111.00 111.00 -30.00 68 12 \w 124.00 175.00 0.50 4.00 -- 111.00 61.00 -90.00 102 13 \w 149.00 175.00 0.50 4.00 -- 111.00 61.00-180.00 52 14 \w 96.00 129.00 0.50 4.00 -- 111.00 45.00 -60.00 66 15 \w 89.00 174.00 0.50 4.00 -- 111.00 61.00-120.00 170 16 \w 89.00 132.00 0.50 4.00 -- 111.00 61.00-180.00 86 17 \w 83.00 111.00 0.50 4.00 -- 111.00 61.00 -90.00 56 18 \w 83.00 176.00 0.50 4.00 -- 111.00 61.00-150.00 186 19 \w 40.00 75.00 0.50 4.00 -- 111.00-111.00 -30.00 70 20 \w 38.00 70.00 0.50 4.00 -- 111.00-111.00 30.00 64 21 \w 36.00 74.00 0.50 4.00 -- 111.00 -77.00 -30.00 76 22 \w 32.00 57.00 0.50 4.00 -- 111.00 -94.00 60.00 50 23 \w 47.00 111.00 0.50 4.00 -- 111.00-111.00 150.00 128 24 \w 35.00 139.00 0.50 4.00 -- 111.00 -77.00 150.00 208 25 \w 138.00 173.00 0.50 4.00 -- 111.00 111.00 150.00 70 26 \w -64.00 31.00 0.50 1.00 -- -41.74 60.00 115.00 190 27 \w -108.00 -18.00 0.50 1.00 -- -41.74 -57.00 -30.00 180 ; _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 -0.0041646667 _diffrn_orient_matrix_UB_12 0.0179637667 _diffrn_orient_matrix_UB_13 -0.0221423333 _diffrn_orient_matrix_UB_21 0.0496374000 _diffrn_orient_matrix_UB_22 0.1244136000 _diffrn_orient_matrix_UB_23 0.0035058000 _diffrn_orient_matrix_UB_31 0.1165809667 _diffrn_orient_matrix_UB_32 0.0165549333 _diffrn_orient_matrix_UB_33 -0.0022729667 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0154 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 85 _diffrn_reflns_limit_l_min -85 _diffrn_reflns_number 33073 _diffrn_reflns_point_group_measured_fraction_full 0.969 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.037 _diffrn_reflns_theta_min 3.861 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.300 _exptl_absorpt_correction_T_max 0.836 _exptl_absorpt_correction_T_min 0.667 _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 1.269 _exptl_crystal_description block _exptl_crystal_F_000 4716 _exptl_crystal_size_max 0.315 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.102 _refine_diff_density_max 0.974 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.087 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.07(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 477 _refine_ls_number_reflns 5261 _refine_ls_number_restraints 433 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0696 _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^)+(0.1504P)^2^+10.6723P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1896 _refine_ls_wR_factor_ref 0.1913 _reflns_Friedel_coverage 0.935 _reflns_Friedel_fraction_full 0.939 _reflns_Friedel_fraction_max 0.936 _reflns_number_gt 5195 _reflns_number_total 5261 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw0944 _cod_original_cell_volume 11653.45(16) _cod_original_sg_symbol_H-M 'R 3 c' _cod_database_code 1577306 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C141F12N21O7P8S4 _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. Twinned data refinement Scales: 0.93(4) 0.07(4) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Uiso/Uaniso restraints and constraints S2A \\sim F2A \\sim F3A \\sim F4A \\sim O2A \\sim O3A \\sim O4A \\sim C23A \\sim S2B \\sim F2B \\sim F3B \\sim F4B \\sim O2B \\sim O3B \\sim O4B \\sim C23B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A N4 \\sim C21 \\sim C22: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A S3B \\sim F5B \\sim F6B \\sim F7B \\sim O5B \\sim O6B \\sim O7B \\sim C24B \\sim S3A \\sim F5A \\sim F6A \\sim F7A \\sim O5A \\sim O6A \\sim O7A \\sim C24A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A Uanis(O2A) = Uanis(O3B) Uanis(O2B) = Uanis(O3B) 4. Others Sof(S2A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(C23A)= 0.33333*(1-FVAR(2)) Sof(S2B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(C23B)= 0.33333*FVAR(2) Sof(S3B)=Sof(F5B)=Sof(F6B)=Sof(F7B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(C24B)= 0.33333*(1-FVAR(3)) Sof(S3A)=Sof(F5A)=Sof(F6A)=Sof(F7A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(C24A)= 0.33333*FVAR(3) Fixed Sof: N3(0.666667) C19(0.666667) C20(0.666667) H20A(0.666667) H20B(0.666667) H20C(0.666667) N4(0.333333) C21(0.333333) C22(0.333333) H22A(0.333333) H22B(0.333333) H22C(0.333333) 5.a Free rotating group: S3B(F5B,F6B,F7B,O5B,O6B,O7B,C24B), S2A(F2A,F3A,F4A,O2A,O3A,O4A,C23A), S2B(F2B, F3B,F4B,O2B,O3B,O4B,C23B), S3A(F5A,F6A,F7A,O5A,O6A,O7A,C24A) 5.b Ternary CH refined with riding coordinates: C6(H6), C9(H9), C12(H12) 5.c Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B) 5.d Idealised Me refined as rotating group: C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C) ; _shelx_res_file ; TITL jjw0944_a.res in R3c jjw0944.res created by SHELXL-2018/3 at 20:28:43 on 11-Jan-2026 REM Old TITL jjw0944 in R3c #161 REM SHELXT solution in R3c REM R1 0.147, Rweak 0.021, Alpha 0.007, Orientation as input REM Flack x = 0.261 ( 0.006 ) from Parsons' quotients REM Formula found by SHELXT: C68 N11 O4B F4A S3A CELL 1.54184 14.027988 14.027988 68.380634 90 90 120 ZERR 6 0.000081 0.000081 0.000517 0 0 0 LATT -3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SYMM -Y,-X,0.5+Z SYMM +Y-X,+Y,0.5+Z SYMM +X,+X-Y,0.5+Z SFAC C H F N O P S UNIT 360 612 54 54 54 24 18 SIMU 0.01 0.02 2 S2A > C23B SIMU 0.01 0.02 2 N4 C21 C22 SIMU 0.01 0.01 2 S3B > C24B S3A > C24A EADP O2A O3B EADP O2B O3B L.S. 10 PLAN 8 TEMP 100 CONF BOND $H LIST 4 MORE -1 fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT -1 3 26 REM REM REM WGHT 0.150400 10.672300 BASF 0.07444 FVAR 0.13007 0.30336 0.67201 P1 6 0.333333 0.666667 0.530339 10.33333 0.02571 0.02571 = 0.02851 0.00000 0.00000 0.01286 P2 6 0.302215 0.510065 0.544490 11.00000 0.03473 0.03029 = 0.03539 0.00344 -0.00173 0.01634 N1 4 0.342256 0.374234 0.520322 11.00000 0.04795 0.03246 = 0.06836 -0.00017 0.00224 0.02528 N2 4 0.224127 0.410138 0.505974 11.00000 0.03874 0.03094 = 0.04400 -0.00634 -0.00022 0.01506 C1 1 0.282425 0.426412 0.522755 11.00000 0.03849 0.02798 = 0.04409 0.00228 0.00282 0.01616 C2 1 0.321719 0.327465 0.502181 11.00000 0.06066 0.03394 = 0.07569 -0.00912 0.00962 0.02331 C3 1 0.249187 0.350106 0.493177 11.00000 0.05547 0.02976 = 0.05761 -0.01145 0.00559 0.01651 C4 1 0.372152 0.263494 0.493713 11.00000 0.08276 0.05366 = 0.11803 -0.02005 0.00680 0.04601 AFIX 137 H4A 2 0.419446 0.258154 0.503259 11.00000 -1.50000 H4B 2 0.414269 0.300650 0.482302 11.00000 -1.50000 H4C 2 0.314834 0.190970 0.490188 11.00000 -1.50000 AFIX 0 C5 1 0.205270 0.318705 0.472775 11.00000 0.07870 0.05433 = 0.05759 -0.02308 -0.00066 0.03195 AFIX 137 H5A 2 0.126302 0.281290 0.473070 11.00000 -1.50000 H5B 2 0.228899 0.270916 0.467300 11.00000 -1.50000 H5C 2 0.232495 0.383806 0.464892 11.00000 -1.50000 AFIX 0 C6 1 0.411089 0.364404 0.536309 11.00000 0.06596 0.04279 = 0.07780 0.00807 0.00278 0.03857 AFIX 13 H6 2 0.402316 0.400909 0.547824 11.00000 -1.20000 AFIX 0 C7 1 0.532491 0.426034 0.531352 11.00000 0.06181 0.07206 = 0.08329 -0.00561 -0.00449 0.04554 AFIX 137 H7A 2 0.545073 0.394379 0.519885 11.00000 -1.50000 H7B 2 0.573685 0.420833 0.542101 11.00000 -1.50000 H7C 2 0.555726 0.501984 0.528927 11.00000 -1.50000 AFIX 0 C8 1 0.365534 0.243973 0.541997 11.00000 0.10082 0.05408 = 0.17769 0.03719 -0.01388 0.04135 AFIX 137 H8A 2 0.291928 0.214258 0.546893 11.00000 -1.50000 H8B 2 0.411231 0.239162 0.551946 11.00000 -1.50000 H8C 2 0.364820 0.202825 0.530725 11.00000 -1.50000 AFIX 0 C9 1 0.136810 0.439406 0.503819 11.00000 0.03933 0.03314 = 0.04530 -0.01056 -0.00739 0.01403 AFIX 13 H9 2 0.139607 0.481337 0.515481 11.00000 -1.20000 AFIX 0 C10 1 0.155761 0.513206 0.486194 11.00000 0.04368 0.05157 = 0.05487 -0.00189 -0.01072 0.01964 AFIX 137 H10A 2 0.231611 0.570222 0.485787 11.00000 -1.50000 H10B 2 0.109878 0.545745 0.487245 11.00000 -1.50000 H10C 2 0.137739 0.470167 0.474442 11.00000 -1.50000 AFIX 0 C11 1 0.023533 0.336437 0.503385 11.00000 0.04082 0.04838 = 0.05940 -0.01373 -0.00247 0.01054 AFIX 137 H11A 2 0.019830 0.290327 0.492697 11.00000 -1.50000 H11B 2 -0.031717 0.357067 0.501726 11.00000 -1.50000 H11C 2 0.011045 0.296978 0.515457 11.00000 -1.50000 AFIX 0 C12 1 0.164841 0.448864 0.556373 11.00000 0.04109 0.03740 = 0.04238 0.00755 0.00293 0.01535 AFIX 13 H12 2 0.115983 0.464866 0.548546 11.00000 -1.20000 AFIX 0 C13 1 0.114110 0.324182 0.558624 11.00000 0.06067 0.03448 = 0.05713 0.01205 0.00985 0.01110 AFIX 23 H13A 2 0.164097 0.308233 0.565821 11.00000 -1.20000 H13B 2 0.102096 0.290216 0.545826 11.00000 -1.20000 AFIX 0 C14 1 0.004262 0.276834 0.569582 11.00000 0.05997 0.04896 = 0.07808 0.01793 0.01572 0.00198 AFIX 23 H14A 2 -0.047567 0.286119 0.561564 11.00000 -1.20000 H14B 2 -0.025247 0.198511 0.571499 11.00000 -1.20000 AFIX 0 C15 1 0.014060 0.330367 0.589233 11.00000 0.06501 0.06415 = 0.05698 0.02436 0.01945 0.01236 AFIX 23 H15A 2 0.056898 0.312217 0.598032 11.00000 -1.20000 H15B 2 -0.058599 0.302368 0.594860 11.00000 -1.20000 AFIX 0 C16 1 0.069465 0.454723 0.586981 11.00000 0.05881 0.06904 = 0.04430 0.00954 0.01736 0.02178 AFIX 23 H16A 2 0.022145 0.473243 0.579520 11.00000 -1.20000 H16B 2 0.080851 0.488571 0.599779 11.00000 -1.20000 AFIX 0 C17 1 0.179461 0.499276 0.576616 11.00000 0.05046 0.04584 = 0.04118 0.01249 0.00640 0.01812 AFIX 23 H17A 2 0.227536 0.482867 0.584325 11.00000 -1.20000 H17B 2 0.214012 0.578628 0.575447 11.00000 -1.20000 AFIX 6 PART -2 S3B 7 -0.015784 0.006267 0.525926 -30.33333 0.08492 0.05070 = 0.15400 -0.00739 0.00974 0.03714 F5B 3 -0.076488 -0.000375 0.562986 -30.33333 0.07649 0.05535 = 0.16093 -0.00297 0.01615 0.04257 F6B 3 0.001065 -0.096651 0.557246 -30.33333 0.07731 0.05988 = 0.16788 -0.00683 0.00948 0.04103 F7B 3 0.098962 0.079889 0.558877 -30.33333 0.08122 0.05585 = 0.17495 -0.00295 0.02125 0.02257 O5B 5 -0.011238 0.111170 0.524276 -30.33333 0.08995 0.03722 = 0.14924 -0.00770 0.00342 0.03654 O6B 5 -0.122326 -0.089370 0.522425 -30.33333 0.08128 0.05135 = 0.15168 -0.00830 0.01497 0.03620 O7B 5 0.076933 0.001842 0.517767 -30.33333 0.09335 0.06296 = 0.15042 -0.01023 0.00785 0.03176 C24B 1 0.002821 -0.003187 0.552546 -30.33333 0.08086 0.05623 = 0.16458 -0.00339 0.01075 0.03802 AFIX 6 PART -1 S2A 7 0.256751 0.682748 0.426994 -20.33333 0.05614 0.06009 = 0.04838 0.00836 -0.00135 0.02165 F2A 3 0.371129 0.580012 0.431589 -20.33333 0.10164 0.10331 = 0.11392 0.00821 -0.00981 0.04442 F3A 3 0.441486 0.711871 0.410644 -20.33333 0.10225 0.12228 = 0.08276 -0.02452 0.03371 0.03709 F4A 3 0.455925 0.748220 0.441436 -20.33333 0.05332 0.11474 = 0.08506 0.01168 -0.01505 0.01987 O2A 5 0.213710 0.646782 0.446443 -20.33333 0.05160 0.06724 = 0.05554 0.01311 -0.00376 0.02035 O3A 5 0.197225 0.605697 0.411440 -20.33333 0.07048 0.09164 = 0.07929 -0.01165 -0.01989 0.03175 O4A 5 0.293698 0.796823 0.422638 -20.33333 0.11920 0.06616 = 0.09519 0.01590 0.00422 0.03565 C23A 1 0.387596 0.680546 0.427733 -20.33333 0.06560 0.07952 = 0.06740 0.00653 0.01460 0.04098 AFIX 6 PART -2 S2B 7 0.327049 0.661010 0.441841 20.33333 0.06020 0.06711 = 0.04809 0.02663 -0.00836 0.03998 F2B 3 0.263995 0.583567 0.405847 20.33333 0.07425 0.09386 = 0.07993 0.02569 -0.02604 0.02938 F3B 3 0.366232 0.759718 0.407228 20.33333 0.07340 0.06074 = 0.04734 0.01274 -0.00535 0.05431 F4B 3 0.438184 0.656651 0.410727 20.33333 0.08010 0.07477 = 0.08276 0.00350 0.01222 0.05325 O2B 5 0.311788 0.554434 0.447126 20.33333 0.05160 0.06724 = 0.05554 0.01311 -0.00376 0.02035 O3B 5 0.229968 0.671553 0.443216 20.33333 0.05160 0.06724 = 0.05554 0.01311 -0.00376 0.02035 O4B 5 0.427936 0.754675 0.448694 20.33333 0.05925 0.08056 = 0.05042 0.02798 -0.00146 0.02952 C23B 1 0.349988 0.665477 0.415170 20.33333 0.06938 0.07523 = 0.06045 0.01116 -0.00017 0.03543 AFIX 6 PART -1 S3A 7 -0.031014 0.050839 0.517367 30.33333 0.07570 0.03480 = 0.13519 -0.00130 0.00727 0.02952 F5A 3 -0.092730 -0.161692 0.515918 30.33333 0.10570 0.06242 = 0.17723 -0.01346 0.01348 0.02182 F6A 3 0.058413 -0.056970 0.500646 30.33333 0.10436 0.07882 = 0.14761 -0.01802 -0.00232 0.04840 F7A 3 0.056629 -0.063411 0.532086 30.33333 0.08587 0.06742 = 0.16382 0.00555 -0.00358 0.04224 O5A 5 -0.094005 0.027857 0.535198 30.33333 0.08859 0.06538 = 0.15253 -0.01187 0.02556 0.03189 O6A 5 -0.091973 0.035197 0.499488 30.33333 0.08173 0.07328 = 0.14832 -0.01026 -0.00565 0.05175 O7A 5 0.077818 0.146868 0.517855 30.33333 0.09346 0.03149 = 0.14587 -0.01121 0.00690 0.02868 C24A 1 -0.000758 -0.063353 0.516456 30.33333 0.08854 0.05255 = 0.15043 -0.01568 0.00679 0.04140 AFIX 0 PART 0 S1 7 0.666667 0.333333 0.479405 10.33333 0.06687 0.06687 = 0.10050 0.00000 0.00000 0.03344 F1 3 0.566388 0.306510 0.444192 11.00000 0.15499 0.15541 = 0.15643 -0.02351 -0.05301 0.08658 O1 5 0.579065 0.222263 0.482440 11.00000 0.07731 0.07513 = 0.10518 0.01113 0.00578 0.04336 C18 1 0.666667 0.333333 0.449380 10.33333 0.08465 0.08465 = 0.13122 0.00000 0.00000 0.04232 PART 1 N3 4 0.271914 0.391567 0.617014 10.66667 0.10139 0.07566 = 0.08055 0.00289 -0.01798 0.04274 C19 1 0.285513 0.320175 0.612574 10.66667 0.07151 0.05564 = 0.06669 0.00205 -0.00977 0.02491 C20 1 0.289184 0.223641 0.609116 10.66667 0.10290 0.07394 = 0.07687 -0.00976 -0.02817 0.03838 AFIX 137 H20A 2 0.251569 0.190646 0.597118 10.66667 -1.50000 H20B 2 0.254027 0.173073 0.619713 10.66667 -1.50000 H20C 2 0.364474 0.241046 0.608149 10.66667 -1.50000 AFIX 0 PART -1 N4 4 0.536550 0.807609 0.624878 10.33333 0.07354 0.05524 = 0.06570 -0.00548 0.00110 0.02706 C21 1 0.445505 0.747397 0.624431 10.33333 0.07335 0.05363 = 0.06076 -0.01338 -0.02075 0.03849 C22 1 0.332916 0.653191 0.623191 10.33333 0.05941 0.06796 = 0.09782 -0.00794 -0.02250 0.04291 AFIX 137 H22A 2 0.301808 0.653575 0.610707 10.33333 -1.50000 H22B 2 0.288770 0.658462 0.633395 10.33333 -1.50000 H22C 2 0.334644 0.586013 0.624662 10.33333 -1.50000 AFIX 0 HKLF 4 REM jjw0944_a.res in R3c REM wR2 = 0.1913, GooF = S = 1.083, Restrained GooF = 1.087 for all data REM R1 = 0.0696 for 5195 Fo > 4sig(Fo) and 0.0701 for all 5261 data REM 477 parameters refined using 433 restraints END WGHT 0.1504 10.6719 REM Highest difference peak 0.974, deepest hole -0.485, 1-sigma level 0.087 Q1 1 0.3180 0.2777 0.5949 11.00000 0.05 0.97 Q2 1 0.0252 -0.0268 0.5111 11.00000 0.05 0.75 Q3 1 -0.0346 0.0558 0.5425 11.00000 0.05 0.63 Q4 1 -0.0202 0.0925 0.5006 11.00000 0.05 0.56 Q5 1 0.3532 0.3369 0.5821 11.00000 0.05 0.52 Q6 1 0.0000 0.0000 0.5403 10.33333 0.05 0.45 Q7 1 0.5477 0.3722 0.4590 11.00000 0.05 0.44 Q8 1 -0.0802 0.0762 0.5284 11.00000 0.05 0.44 ; _shelx_res_checksum 31256 _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 1.187 _oxdiff_exptl_absorpt_empirical_full_min 0.852 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' '-x+y, y, z+1/2' 'x, x-y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' 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 P1 P 0.333333 0.666667 0.53034(2) 0.0266(3) Uani 1 3 d S T P . . P2 P 0.30221(8) 0.51007(8) 0.54449(2) 0.0334(3) Uani 1 1 d . . . . . N1 N 0.3423(4) 0.3742(3) 0.52032(8) 0.0473(10) Uani 1 1 d . . . . . N2 N 0.2241(3) 0.4101(3) 0.50597(6) 0.0389(8) Uani 1 1 d . . . . . C1 C 0.2824(4) 0.4264(3) 0.52276(7) 0.0371(9) Uani 1 1 d . . . . . C2 C 0.3217(5) 0.3275(4) 0.50218(10) 0.0569(14) Uani 1 1 d . . . . . C3 C 0.2492(5) 0.3501(4) 0.49318(9) 0.0497(12) Uani 1 1 d . . . . . C4 C 0.3722(7) 0.2635(6) 0.49371(15) 0.080(2) Uani 1 1 d . . . . . H4A H 0.419446 0.258154 0.503259 0.119 Uiso 1 1 calc R U . . . H4B H 0.414269 0.300650 0.482302 0.119 Uiso 1 1 calc R U . . . H4C H 0.314834 0.190970 0.490188 0.119 Uiso 1 1 calc R U . . . C5 C 0.2053(6) 0.3187(6) 0.47277(10) 0.0641(16) Uani 1 1 d . . . . . H5A H 0.126302 0.281290 0.473070 0.096 Uiso 1 1 calc R U . . . H5B H 0.228899 0.270916 0.467300 0.096 Uiso 1 1 calc R U . . . H5C H 0.232495 0.383806 0.464892 0.096 Uiso 1 1 calc R U . . . C6 C 0.4111(6) 0.3644(5) 0.53631(10) 0.0571(14) Uani 1 1 d . . . . . H6 H 0.402316 0.400909 0.547824 0.069 Uiso 1 1 calc R U . . . C7 C 0.5325(6) 0.4260(7) 0.53135(12) 0.0670(16) Uani 1 1 d . . . . . H7A H 0.545073 0.394379 0.519885 0.101 Uiso 1 1 calc R U . . . H7B H 0.573685 0.420833 0.542101 0.101 Uiso 1 1 calc R U . . . H7C H 0.555726 0.501984 0.528927 0.101 Uiso 1 1 calc R U . . . C8 C 0.3655(10) 0.2440(7) 0.5420(2) 0.110(4) Uani 1 1 d . . . . . H8A H 0.291928 0.214258 0.546893 0.165 Uiso 1 1 calc R U . . . H8B H 0.411231 0.239162 0.551946 0.165 Uiso 1 1 calc R U . . . H8C H 0.364820 0.202825 0.530725 0.165 Uiso 1 1 calc R U . . . C9 C 0.1368(4) 0.4394(4) 0.50382(7) 0.0411(9) Uani 1 1 d . . . . . H9 H 0.139607 0.481337 0.515481 0.049 Uiso 1 1 calc R U . . . C10 C 0.1558(5) 0.5132(5) 0.48619(9) 0.0519(12) Uani 1 1 d . . . . . H10A H 0.231611 0.570222 0.485787 0.078 Uiso 1 1 calc R U . . . H10B H 0.109878 0.545745 0.487245 0.078 Uiso 1 1 calc R U . . . H10C H 0.137739 0.470167 0.474442 0.078 Uiso 1 1 calc R U . . . C11 C 0.0235(4) 0.3364(5) 0.50338(9) 0.0548(13) Uani 1 1 d . . . . . H11A H 0.019830 0.290327 0.492697 0.082 Uiso 1 1 calc R U . . . H11B H -0.031717 0.357067 0.501726 0.082 Uiso 1 1 calc R U . . . H11C H 0.011045 0.296978 0.515457 0.082 Uiso 1 1 calc R U . . . C12 C 0.1648(4) 0.4489(4) 0.55637(7) 0.0422(10) Uani 1 1 d . . . . . H12 H 0.115983 0.464866 0.548546 0.051 Uiso 1 1 calc R U . . . C13 C 0.1141(5) 0.3242(4) 0.55862(9) 0.0564(13) Uani 1 1 d . . . . . H13A H 0.164097 0.308233 0.565821 0.068 Uiso 1 1 calc R U . . . H13B H 0.102096 0.290216 0.545826 0.068 Uiso 1 1 calc R U . . . C14 C 0.0043(6) 0.2768(6) 0.56958(12) 0.074(2) Uani 1 1 d . . . . . H14A H -0.047567 0.286119 0.561564 0.088 Uiso 1 1 calc R U . . . H14B H -0.025247 0.198511 0.571499 0.088 Uiso 1 1 calc R U . . . C15 C 0.0141(6) 0.3304(6) 0.58923(10) 0.0709(18) Uani 1 1 d . . . . . H15A H 0.056898 0.312217 0.598032 0.085 Uiso 1 1 calc R U . . . H15B H -0.058599 0.302368 0.594860 0.085 Uiso 1 1 calc R U . . . C16 C 0.0695(6) 0.4547(6) 0.58698(9) 0.0619(15) Uani 1 1 d . . . . . H16A H 0.022145 0.473243 0.579520 0.074 Uiso 1 1 calc R U . . . H16B H 0.080851 0.488571 0.599779 0.074 Uiso 1 1 calc R U . . . C17 C 0.1795(5) 0.4993(4) 0.57662(8) 0.0485(11) Uani 1 1 d . . . . . H17A H 0.227536 0.482867 0.584325 0.058 Uiso 1 1 calc R U . . . H17B H 0.214012 0.578628 0.575447 0.058 Uiso 1 1 calc R U . . . S3B S -0.016(3) 0.006(3) 0.5259(3) 0.095(4) Uani 0.109(4) 1 d G U P A -2 F5B F -0.076(6) 0.000(6) 0.5630(4) 0.093(7) Uani 0.109(4) 1 d G U P A -2 F6B F 0.001(6) -0.097(6) 0.5572(6) 0.099(8) Uani 0.109(4) 1 d G U P A -2 F7B F 0.099(5) 0.080(6) 0.5589(7) 0.109(12) Uani 0.109(4) 1 d G U P A -2 O5B O -0.011(4) 0.111(4) 0.5243(6) 0.090(6) Uani 0.109(4) 1 d G U P A -2 O6B O -0.122(3) -0.089(4) 0.5224(8) 0.093(6) Uani 0.109(4) 1 d G U P A -2 O7B O 0.077(4) 0.002(4) 0.5178(5) 0.105(6) Uani 0.109(4) 1 d G U P A -2 C24B C 0.003(4) -0.003(5) 0.5525(3) 0.099(6) Uani 0.109(4) 1 d G U P A -2 S2A S 0.2568(5) 0.6827(6) 0.42699(9) 0.0582(16) Uani 0.232(4) 1 d G U P B -1 F2A F 0.3711(13) 0.5800(14) 0.4316(3) 0.109(6) Uani 0.232(4) 1 d G U P B -1 F3A F 0.4415(11) 0.7119(18) 0.4106(3) 0.111(8) Uani 0.232(4) 1 d G U P B -1 F4A F 0.4559(8) 0.7482(16) 0.4414(3) 0.094(8) Uani 0.232(4) 1 d G U P B -1 O2A O 0.2137(10) 0.6468(14) 0.44644(13) 0.062(4) Uani 0.232(4) 1 d G U P B -1 O3A O 0.1972(10) 0.6057(13) 0.41144(19) 0.084(7) Uani 0.232(4) 1 d G U P B -1 O4A O 0.2937(12) 0.7968(7) 0.4226(3) 0.098(8) Uani 0.232(4) 1 d G U P B -1 C23A C 0.3876(6) 0.6805(11) 0.4277(2) 0.069(5) Uani 0.232(4) 1 d G U P B -1 S2B S 0.327(2) 0.661(3) 0.44184(15) 0.055(3) Uani 0.101(4) 1 d G U P B -2 F2B F 0.264(3) 0.584(5) 0.4058(4) 0.088(13) Uani 0.101(4) 1 d G U P B -2 F3B F 0.366(3) 0.760(4) 0.4072(4) 0.051(6) Uani 0.101(4) 1 d G U P B -2 F4B F 0.438(3) 0.657(4) 0.4107(4) 0.073(8) Uani 0.101(4) 1 d G U P B -2 O2B O 0.312(3) 0.554(3) 0.4471(5) 0.062(4) Uani 0.101(4) 1 d G U P B -2 O3B O 0.230(3) 0.672(4) 0.4432(3) 0.062(4) Uani 0.101(4) 1 d G U P B -2 O4B O 0.428(3) 0.755(3) 0.4487(4) 0.066(11) Uani 0.101(4) 1 d G U P B -2 C23B C 0.350(3) 0.665(4) 0.41517(17) 0.069(6) Uani 0.101(4) 1 d G U P B -2 S3A S -0.0310(7) 0.0508(6) 0.51737(17) 0.081(2) Uani 0.224(4) 1 d G U P A -1 F5A F -0.0927(14) -0.1617(5) 0.5159(3) 0.124(7) Uani 0.224(4) 1 d G U P A -1 F6A F 0.0584(15) -0.0570(13) 0.5006(3) 0.109(6) Uani 0.224(4) 1 d G U P A -1 F7A F 0.0566(16) -0.0634(13) 0.5321(3) 0.104(4) Uani 0.224(4) 1 d G U P A -1 O5A O -0.0940(14) 0.0279(12) 0.5352(2) 0.105(5) Uani 0.224(4) 1 d G U P A -1 O6A O -0.0920(13) 0.0352(12) 0.4995(2) 0.095(6) Uani 0.224(4) 1 d G U P A -1 O7A O 0.0778(9) 0.1469(6) 0.5179(3) 0.091(5) Uani 0.224(4) 1 d G U P A -1 C24A C -0.0008(11) -0.0634(7) 0.5165(2) 0.094(5) Uani 0.224(4) 1 d G U P A -1 S1 S 0.666667 0.333333 0.47940(7) 0.0781(9) Uani 1 3 d S T P . . F1 F 0.5664(9) 0.3065(9) 0.44419(17) 0.152(4) Uani 1 1 d . . . . . O1 O 0.5791(5) 0.2223(5) 0.48244(11) 0.0835(16) Uani 1 1 d . . . . . C18 C 0.666667 0.333333 0.4494(4) 0.100(5) Uani 1 3 d S T P . . N3 N 0.2719(11) 0.3916(10) 0.61701(18) 0.087(3) Uani 0.6667 1 d . . P C 1 C19 C 0.2855(10) 0.3202(9) 0.61257(17) 0.068(2) Uani 0.6667 1 d . . P C 1 C20 C 0.2892(14) 0.2236(11) 0.6091(2) 0.087(4) Uani 0.6667 1 d . . P C 1 H20A H 0.251569 0.190646 0.597118 0.131 Uiso 0.6667 1 calc R U P C 1 H20B H 0.254027 0.173073 0.619713 0.131 Uiso 0.6667 1 calc R U P C 1 H20C H 0.364474 0.241046 0.608149 0.131 Uiso 0.6667 1 calc R U P C 1 N4 N 0.5365(17) 0.8076(15) 0.6249(3) 0.067(4) Uani 0.3333 1 d . U P D -1 C21 C 0.4455(19) 0.7474(17) 0.6244(3) 0.060(4) Uani 0.3333 1 d . U P D -1 C22 C 0.333(8) 0.653(6) 0.6232(4) 0.070(10) Uani 0.3333 1 d . U P D -1 H22A H 0.301808 0.653575 0.610707 0.105 Uiso 0.3333 1 calc R U P D -1 H22B H 0.288770 0.658462 0.633395 0.105 Uiso 0.3333 1 calc R U P D -1 H22C H 0.334644 0.586013 0.624662 0.105 Uiso 0.3333 1 calc R U P D -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0257(5) 0.0257(5) 0.0285(7) 0.000 0.000 0.0129(2) P2 0.0347(5) 0.0303(5) 0.0354(5) 0.0034(4) -0.0017(4) 0.0163(4) N1 0.048(2) 0.0325(18) 0.068(3) -0.0002(17) 0.0022(19) 0.0253(17) N2 0.0387(18) 0.0309(17) 0.0440(19) -0.0063(14) -0.0002(15) 0.0151(15) C1 0.038(2) 0.0280(18) 0.044(2) 0.0023(15) 0.0028(17) 0.0162(16) C2 0.061(3) 0.034(2) 0.076(4) -0.009(2) 0.010(3) 0.023(2) C3 0.055(3) 0.030(2) 0.058(3) -0.0115(19) 0.006(2) 0.017(2) C4 0.083(5) 0.054(3) 0.118(7) -0.020(4) 0.007(4) 0.046(4) C5 0.079(4) 0.054(3) 0.058(3) -0.023(3) -0.001(3) 0.032(3) C6 0.066(3) 0.043(3) 0.078(4) 0.008(2) 0.003(3) 0.039(3) C7 0.062(3) 0.072(4) 0.083(4) -0.006(3) -0.004(3) 0.046(3) C8 0.101(7) 0.054(4) 0.178(12) 0.037(5) -0.014(7) 0.041(4) C9 0.039(2) 0.033(2) 0.045(2) -0.0106(17) -0.0074(17) 0.0140(17) C10 0.044(2) 0.052(3) 0.055(3) -0.002(2) -0.011(2) 0.020(2) C11 0.041(3) 0.048(3) 0.059(3) -0.014(2) -0.002(2) 0.011(2) C12 0.041(2) 0.037(2) 0.042(2) 0.0075(17) 0.0029(17) 0.0154(18) C13 0.061(3) 0.034(2) 0.057(3) 0.012(2) 0.010(2) 0.011(2) C14 0.060(4) 0.049(3) 0.078(4) 0.018(3) 0.016(3) 0.002(3) C15 0.065(4) 0.064(4) 0.057(3) 0.024(3) 0.019(3) 0.012(3) C16 0.059(3) 0.069(4) 0.044(3) 0.010(2) 0.017(2) 0.022(3) C17 0.050(3) 0.046(3) 0.041(2) 0.0125(19) 0.006(2) 0.018(2) S3B 0.085(7) 0.051(5) 0.154(7) -0.007(6) 0.010(6) 0.037(5) F5B 0.076(12) 0.055(10) 0.161(13) -0.003(12) 0.016(12) 0.043(9) F6B 0.077(12) 0.060(11) 0.168(14) -0.007(12) 0.009(12) 0.041(10) F7B 0.081(17) 0.056(15) 0.175(18) -0.003(16) 0.021(17) 0.023(14) O5B 0.090(9) 0.037(8) 0.149(10) -0.008(8) 0.003(9) 0.037(8) O6B 0.081(9) 0.051(7) 0.152(9) -0.008(8) 0.015(8) 0.036(7) O7B 0.093(9) 0.063(8) 0.150(9) -0.010(8) 0.008(8) 0.032(7) C24B 0.081(10) 0.056(9) 0.165(11) -0.003(10) 0.011(10) 0.038(9) S2A 0.056(3) 0.060(4) 0.048(3) 0.008(3) -0.001(2) 0.022(3) F2A 0.102(11) 0.103(11) 0.114(12) 0.008(11) -0.010(11) 0.044(10) F3A 0.102(12) 0.122(14) 0.083(11) -0.025(12) 0.034(10) 0.037(11) F4A 0.053(10) 0.115(14) 0.085(13) 0.012(12) -0.015(9) 0.020(10) O2A 0.052(7) 0.067(9) 0.056(7) 0.013(7) -0.004(6) 0.020(7) O3A 0.070(12) 0.092(14) 0.079(12) -0.012(11) -0.020(10) 0.032(11) O4A 0.119(16) 0.066(12) 0.095(15) 0.016(11) 0.004(13) 0.036(12) C23A 0.066(7) 0.080(8) 0.067(7) 0.007(7) 0.015(7) 0.041(7) S2B 0.060(6) 0.067(7) 0.048(4) 0.027(6) -0.008(7) 0.040(6) F2B 0.074(19) 0.09(2) 0.080(19) 0.026(17) -0.026(17) 0.029(17) F3B 0.073(12) 0.061(11) 0.047(11) 0.013(10) -0.005(10) 0.054(9) F4B 0.080(14) 0.075(14) 0.083(14) 0.004(14) 0.012(13) 0.053(12) O2B 0.052(7) 0.067(9) 0.056(7) 0.013(7) -0.004(6) 0.020(7) O3B 0.052(7) 0.067(9) 0.056(7) 0.013(7) -0.004(6) 0.020(7) O4B 0.059(16) 0.081(17) 0.050(16) 0.028(14) -0.001(14) 0.030(14) C23B 0.069(8) 0.075(8) 0.060(7) 0.011(8) 0.000(8) 0.035(8) S3A 0.076(5) 0.035(3) 0.135(6) -0.001(4) 0.007(4) 0.030(3) F5A 0.106(11) 0.062(9) 0.177(13) -0.013(10) 0.013(11) 0.022(9) F6A 0.104(11) 0.079(9) 0.148(12) -0.018(9) -0.002(10) 0.048(8) F7A 0.086(8) 0.067(7) 0.164(10) 0.006(8) -0.004(8) 0.042(6) O5A 0.089(8) 0.065(7) 0.153(9) -0.012(7) 0.026(8) 0.032(7) O6A 0.082(11) 0.073(10) 0.148(14) -0.010(11) -0.006(11) 0.052(9) O7A 0.093(9) 0.031(6) 0.146(10) -0.011(8) 0.007(9) 0.029(6) C24A 0.089(8) 0.053(7) 0.150(9) -0.016(7) 0.007(7) 0.041(6) S1 0.0669(11) 0.0669(11) 0.100(2) 0.000 0.000 0.0334(6) F1 0.155(7) 0.155(8) 0.156(9) -0.024(6) -0.053(6) 0.087(7) O1 0.077(3) 0.075(3) 0.105(5) 0.011(3) 0.006(3) 0.043(3) C18 0.085(6) 0.085(6) 0.131(16) 0.000 0.000 0.042(3) N3 0.101(8) 0.076(7) 0.081(6) 0.003(5) -0.018(6) 0.043(6) C19 0.072(6) 0.056(5) 0.067(6) 0.002(4) -0.010(5) 0.025(5) C20 0.103(10) 0.074(7) 0.077(7) -0.010(6) -0.028(7) 0.038(7) N4 0.074(11) 0.055(8) 0.066(9) -0.005(7) 0.001(8) 0.027(8) C21 0.073(11) 0.054(8) 0.061(9) -0.013(7) -0.021(8) 0.038(9) C22 0.059(15) 0.07(2) 0.098(11) -0.008(18) -0.02(2) 0.043(16) 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' 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 0 0 3 0.0509 0 0 -3 0.0509 1 -1 2 0.1300 1 0 -2 0.1046 0 -1 -2 0.1027 -1 1 -2 0.0752 -9 3 0 0.1270 -1 8 15 0.1351 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 P2 P1 P2 102.64(6) 3_565 2_665 ? P2 P1 P2 102.64(6) 2_665 . ? P2 P1 P2 102.64(6) 3_565 . ? C1 P2 P1 99.87(15) . . ? C1 P2 C12 105.6(2) . . ? C12 P2 P1 106.92(16) . . ? C1 N1 C6 123.4(5) . . ? C2 N1 C1 109.2(5) . . ? C2 N1 C6 127.2(5) . . ? C1 N2 C3 108.8(4) . . ? C1 N2 C9 123.3(4) . . ? C3 N2 C9 127.3(4) . . ? N1 C1 P2 120.3(4) . . ? N2 C1 P2 132.8(4) . . ? N2 C1 N1 106.6(4) . . ? N1 C2 C4 125.8(7) . . ? C3 C2 N1 107.6(5) . . ? C3 C2 C4 126.5(7) . . ? N2 C3 C5 125.3(5) . . ? C2 C3 N2 107.8(5) . . ? C2 C3 C5 126.9(5) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 H6 106.3 . . ? N1 C6 C7 112.0(5) . . ? N1 C6 C8 110.6(7) . . ? C7 C6 H6 106.3 . . ? C7 C6 C8 114.7(6) . . ? C8 C6 H6 106.3 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9 107.2 . . ? N2 C9 C10 112.3(4) . . ? N2 C9 C11 110.8(4) . . ? C10 C9 H9 107.2 . . ? C11 C9 H9 107.2 . . ? C11 C9 C10 112.0(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12 109.7 . . ? C13 C12 P2 110.7(4) . . ? C13 C12 H12 109.7 . . ? C17 C12 P2 108.4(4) . . ? C17 C12 H12 109.7 . . ? C17 C12 C13 108.5(4) . . ? C12 C13 H13A 109.7 . . ? C12 C13 H13B 109.7 . . ? C12 C13 C14 109.6(6) . . ? H13A C13 H13B 108.2 . . ? C14 C13 H13A 109.7 . . ? C14 C13 H13B 109.7 . . ? C13 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C15 C14 C13 113.4(6) . . ? C15 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C14 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C14 C15 C16 110.3(5) . . ? H15A C15 H15B 108.1 . . ? C16 C15 H15A 109.6 . . ? C16 C15 H15B 109.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C17 C16 C15 110.5(6) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C12 C17 H17A 109.4 . . ? C12 C17 H17B 109.4 . . ? C16 C17 C12 111.1(5) . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O5B S3B C24B 102.3 . . ? O6B S3B O5B 115.5 . . ? O6B S3B O7B 115.58(7) . . ? O6B S3B C24B 102.34(8) . . ? O7B S3B O5B 115.5 . . ? O7B S3B C24B 102.4 . . ? F5B C24B S3B 111.9 . . ? F6B C24B S3B 111.8 . . ? F6B C24B F5B 107.0 . . ? F6B C24B F7B 106.99(8) . . ? F7B C24B S3B 111.83(9) . . ? F7B C24B F5B 106.99(9) . . ? O2A S2A O3A 115.6 . . ? O2A S2A O4A 115.6 . . ? O2A S2A C23A 102.4 . . ? O3A S2A C23A 102.4 . . ? O4A S2A O3A 115.4 . . ? O4A S2A C23A 102.4 . . ? F2A C23A S2A 111.9 . . ? F2A C23A F3A 106.8 . . ? F2A C23A F4A 107.2 . . ? F3A C23A S2A 111.8 . . ? F4A C23A S2A 111.8 . . ? F4A C23A F3A 106.9 . . ? O2B S2B C23B 102.4 . . ? O3B S2B O2B 115.45(5) . . ? O3B S2B O4B 115.5 . . ? O3B S2B C23B 102.6 . . ? O4B S2B O2B 115.5 . . ? O4B S2B C23B 102.38(7) . . ? F2B C23B S2B 111.94(6) . . ? F3B C23B S2B 112.0 . . ? F3B C23B F2B 106.82(5) . . ? F4B C23B S2B 112.0 . . ? F4B C23B F2B 106.86(6) . . ? F4B C23B F3B 106.9 . . ? O5A S3A O6A 115.5 . . ? O5A S3A O7A 115.6 . . ? O5A S3A C24A 102.4 . . ? O6A S3A O7A 115.5 . . ? O6A S3A C24A 102.4 . . ? O7A S3A C24A 102.4 . . ? F5A C24A S3A 111.9 . . ? F5A C24A F6A 107.0 . . ? F5A C24A F7A 107.0 . . ? F6A C24A S3A 111.8 . . ? F7A C24A S3A 111.8 . . ? F7A C24A F6A 107.0 . . ? O1 S1 O1 117.95(17) . 3_665 ? O1 S1 O1 117.95(17) . 2_655 ? O1 S1 O1 117.96(17) 2_655 3_665 ? O1 S1 C18 98.3(3) 3_665 . ? O1 S1 C18 98.3(3) . . ? O1 S1 C18 98.3(3) 2_655 . ? F1 C18 S1 105.7(13) . . ? F1 C18 S1 105.7(13) 3_665 . ? F1 C18 S1 105.7(13) 2_655 . ? F1 C18 F1 113.0(11) 3_665 . ? F1 C18 F1 113.0(11) 2_655 . ? F1 C18 F1 113.0(11) 2_655 3_665 ? N3 C19 C20 171.4(15) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C22 169(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 P1 P2 2.2346(12) 3_565 ? P1 P2 2.2346(12) 2_665 ? P1 P2 2.2347(12) . ? P2 C1 1.827(5) . ? P2 C12 1.859(5) . ? N1 C1 1.372(6) . ? N1 C2 1.365(8) . ? N1 C6 1.510(8) . ? N2 C1 1.360(6) . ? N2 C3 1.376(6) . ? N2 C9 1.481(7) . ? C2 C3 1.356(10) . ? C2 C4 1.509(7) . ? C3 C5 1.500(9) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6 0.9800 . ? C6 C7 1.513(10) . ? C6 C8 1.528(9) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9 0.9800 . ? C9 C10 1.523(8) . ? C9 C11 1.522(7) . ? 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 H12 0.9800 . ? C12 C13 1.531(7) . ? C12 C17 1.521(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.534(9) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.512(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.522(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.520(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? S3B O5B 1.4452 . ? S3B O6B 1.4442(14) . ? S3B O7B 1.4448 . ? S3B C24B 1.8530 . ? F5B C24B 1.3390 . ? F6B C24B 1.3381 . ? F7B C24B 1.339(2) . ? S2A O2A 1.4433 . ? S2A O3A 1.4472 . ? S2A O4A 1.4452 . ? S2A C23A 1.8518 . ? F2A C23A 1.3364 . ? F3A C23A 1.3409 . ? F4A C23A 1.3372 . ? S2B O2B 1.4462 . ? S2B O3B 1.4446 . ? S2B O4B 1.4455(10) . ? S2B C23B 1.8476 . ? F2B C23B 1.3401(12) . ? F3B C23B 1.3391 . ? F4B C23B 1.3385 . ? S3A O5A 1.4445 . ? S3A O6A 1.4445 . ? S3A O7A 1.4457 . ? S3A C24A 1.8520 . ? F5A C24A 1.3376 . ? F6A C24A 1.3385 . ? F7A C24A 1.3383 . ? S1 O1 1.437(6) 2_655 ? S1 O1 1.437(7) . ? S1 O1 1.437(6) 3_665 ? S1 C18 2.05(3) . ? F1 C18 1.310(13) . ? N3 C19 1.150(18) . ? C19 C20 1.401(19) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? N4 C21 1.13(3) . ? C21 C22 1.47(10) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 P1 P2 C1 N1 127.2(3) . . . . ? P1 P2 C1 N2 -45.0(5) . . . . ? P1 P2 C12 C13 155.5(4) . . . . ? P1 P2 C12 C17 -85.6(3) . . . . ? P2 C12 C13 C14 176.5(5) . . . . ? P2 C12 C17 C16 178.6(4) . . . . ? N1 C2 C3 N2 -0.7(6) . . . . ? N1 C2 C3 C5 177.9(6) . . . . ? C1 P2 C12 C13 49.8(4) . . . . ? C1 P2 C12 C17 168.6(3) . . . . ? C1 N1 C2 C3 0.0(6) . . . . ? C1 N1 C2 C4 179.3(6) . . . . ? C1 N1 C6 C7 -115.3(6) . . . . ? C1 N1 C6 C8 115.5(8) . . . . ? C1 N2 C3 C2 1.1(6) . . . . ? C1 N2 C3 C5 -177.5(5) . . . . ? C1 N2 C9 C10 126.4(5) . . . . ? C1 N2 C9 C11 -107.6(5) . . . . ? C2 N1 C1 P2 -173.4(4) . . . . ? C2 N1 C1 N2 0.6(5) . . . . ? C2 N1 C6 C7 70.3(7) . . . . ? C2 N1 C6 C8 -58.9(9) . . . . ? C3 N2 C1 P2 172.0(4) . . . . ? C3 N2 C1 N1 -1.0(5) . . . . ? C3 N2 C9 C10 -63.5(6) . . . . ? C3 N2 C9 C11 62.5(7) . . . . ? C4 C2 C3 N2 -180.0(6) . . . . ? C4 C2 C3 C5 -1.4(10) . . . . ? C6 N1 C1 P2 11.3(6) . . . . ? C6 N1 C1 N2 -174.7(5) . . . . ? C6 N1 C2 C3 175.1(5) . . . . ? C6 N1 C2 C4 -5.6(10) . . . . ? C9 N2 C1 P2 -16.3(7) . . . . ? C9 N2 C1 N1 170.7(4) . . . . ? C9 N2 C3 C2 -170.2(5) . . . . ? C9 N2 C3 C5 11.2(9) . . . . ? C12 P2 C1 N1 -122.0(4) . . . . ? C12 P2 C1 N2 65.8(5) . . . . ? C12 C13 C14 C15 -55.8(8) . . . . ? C13 C12 C17 C16 -61.1(6) . . . . ? C13 C14 C15 C16 53.6(9) . . . . ? C14 C15 C16 C17 -54.5(8) . . . . ? C15 C16 C17 C12 59.8(7) . . . . ? C17 C12 C13 C14 57.7(7) . . . . ? O5B S3B C24B F5B 59.97(9) . . . . ? O5B S3B C24B F6B 180.0 . . . . ? O5B S3B C24B F7B -60.0 . . . . ? O6B S3B C24B F5B -60.01(11) . . . . ? O6B S3B C24B F6B 60.0 . . . . ? O6B S3B C24B F7B 180.0 . . . . ? O7B S3B C24B F5B 179.96(11) . . . . ? O7B S3B C24B F6B -60.02(7) . . . . ? O7B S3B C24B F7B 59.9 . . . . ? O2A S2A C23A F2A 60.1 . . . . ? O2A S2A C23A F3A 179.9 . . . . ? O2A S2A C23A F4A -60.2 . . . . ? O3A S2A C23A F2A -59.9 . . . . ? O3A S2A C23A F3A 59.9 . . . . ? O3A S2A C23A F4A 179.8 . . . . ? O4A S2A C23A F2A -179.8 . . . . ? O4A S2A C23A F3A -60.0 . . . . ? O4A S2A C23A F4A 59.9 . . . . ? O2B S2B C23B F2B 60.0 . . . . ? O2B S2B C23B F3B 180.0 . . . . ? O2B S2B C23B F4B -59.95(7) . . . . ? O3B S2B C23B F2B -60.0 . . . . ? O3B S2B C23B F3B 60.0 . . . . ? O3B S2B C23B F4B -179.95(7) . . . . ? O4B S2B C23B F2B 180.0 . . . . ? O4B S2B C23B F3B -60.0 . . . . ? O4B S2B C23B F4B 60.01(7) . . . . ? O5A S3A C24A F5A 59.9 . . . . ? O5A S3A C24A F6A -180.0 . . . . ? O5A S3A C24A F7A -60.0 . . . . ? O6A S3A C24A F5A -60.1 . . . . ? O6A S3A C24A F6A 60.0 . . . . ? O6A S3A C24A F7A 180.0 . . . . ? O7A S3A C24A F5A 180.0 . . . . ? O7A S3A C24A F6A -59.9 . . . . ? O7A S3A C24A F7A 60.0 . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.93(4) 2 0.07(4) 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 -0.0000 0.0000 3.0000 -0.0664 0.0105 -0.0068 0.0000 -0.0000 -3.0000 0.0664 -0.0105 0.0068 1.0000 -1.0000 2.0000 -0.0664 -0.0678 0.0955 1.0000 0.0000 -2.0000 0.0401 0.0426 0.1211 0.0000 -1.0000 -2.0000 0.0263 -0.1314 -0.0120 -1.0000 1.0000 -2.0000 0.0664 0.0678 -0.0955 -9.0000 3.0000 0.0000 0.0914 -0.0735 -0.9996 -1.0000 8.0000 15.0000 -0.1843 0.9983 -0.0182