#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577313.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_1577313 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 'C H2 Cl2, C F3 O3 S, C34 H62 N4 P3' _chemical_formula_sum 'C36 H64 Cl2 F3 N4 O3 P3 S' _chemical_formula_weight 853.78 _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 dual _audit_creation_date 2021-01-22 _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.1790(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.24000(10) _cell_length_b 14.58910(10) _cell_length_c 17.7842(2) _cell_measurement_reflns_used 28702 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.5670 _cell_measurement_theta_min 3.0230 _cell_volume 4447.03(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.5700 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _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 -70.00 12.00 0.50 3.00 -- -38.50 94.00 131.00 164 2 \w 24.00 77.00 0.50 3.00 -- 42.75 -94.00 20.00 106 3 \w 71.00 107.00 0.50 12.00 -- 111.00 -94.00 20.00 72 4 \w 105.00 177.00 0.50 12.00 -- 111.00 94.00 131.00 144 5 \w -110.00 -24.00 0.50 3.00 -- -38.50 -38.00 -30.00 172 6 \w -103.00 -14.00 0.50 3.00 -- -38.50 -57.00-120.00 178 7 \w -50.00 -6.00 0.50 3.00 -- -38.50 125.00 30.00 88 8 \w 28.00 55.00 0.50 3.00 -- 42.75-125.00-150.00 54 9 \w 86.00 113.00 0.50 3.00 -- 42.75 57.00 -90.00 54 10 \w 16.00 48.00 0.50 3.00 -- 42.75 57.00 -90.00 64 11 \w 40.00 65.00 0.50 12.00 -- 111.00-125.00 30.00 50 12 \w 99.00 169.00 0.50 12.00 -- 111.00 125.00-180.00 140 13 \w 59.00 121.00 0.50 12.00 -- 111.00 -30.00 0.00 124 14 \w 101.00 146.00 0.50 12.00 -- 111.00 30.00 -60.00 90 15 \w 71.00 107.00 0.50 12.00 -- 111.00 -94.00 -60.00 72 16 \w 50.00 88.00 0.50 12.00 -- 111.00 -94.00 150.00 76 17 \w 40.00 112.00 0.50 12.00 -- 111.00-125.00-180.00 144 18 \w 83.00 109.00 0.50 12.00 -- 111.00-125.00 30.00 52 19 \w 42.00 138.00 0.50 12.00 -- 111.00 -61.00-180.00 192 20 \w 123.00 159.00 0.50 12.00 -- 111.00 45.00-180.00 72 21 \w 44.00 72.00 0.50 12.00 -- 111.00 -61.00 0.00 56 22 \w 126.00 171.00 0.50 12.00 -- 111.00 77.00 0.00 90 23 \w 82.00 109.00 0.50 12.00 -- 111.00-112.00 -57.90 54 24 \w 67.00 176.00 0.50 12.00 -- 111.00 15.00 90.00 218 25 \w 55.00 107.00 0.50 12.00 -- 111.00 -94.00 90.00 104 26 \w 30.00 105.00 0.50 12.00 -- 111.00 -94.00 0.00 150 27 \w 65.00 112.00 0.50 12.00 -- 111.00-125.00 150.00 94 28 \w 40.00 65.00 0.50 12.00 -- 111.00 -94.00 60.00 50 29 \w 80.00 105.00 0.50 12.00 -- 111.00 -94.00 60.00 50 30 \w 122.00 171.00 0.50 12.00 -- 111.00 45.00 -60.00 98 31 \w 49.00 95.00 0.50 12.00 -- 111.00-125.00 0.00 92 32 \w 92.00 135.00 0.50 12.00 -- 111.00 -45.00 60.00 86 33 \w 40.00 66.00 0.50 12.00 -- 111.00-125.00 -60.00 52 34 \w 83.00 110.00 0.50 12.00 -- 111.00-125.00 -60.00 54 35 \w 38.00 107.00 0.50 12.00 -- 111.00 -94.00-180.00 138 36 \w 54.00 81.00 0.50 12.00 -- 111.00-133.00-107.64 54 37 \w 83.00 118.00 0.50 12.00 -- 111.00-133.00-107.64 70 38 \w 70.00 95.00 0.50 12.00 -- 111.00 -30.00 150.00 50 ; _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 0.0443396000 _diffrn_orient_matrix_UB_12 -0.0900083000 _diffrn_orient_matrix_UB_13 0.0194927000 _diffrn_orient_matrix_UB_21 -0.0298495000 _diffrn_orient_matrix_UB_22 -0.0003009000 _diffrn_orient_matrix_UB_23 0.0786264000 _diffrn_orient_matrix_UB_31 -0.0722572000 _diffrn_orient_matrix_UB_32 -0.0551791000 _diffrn_orient_matrix_UB_33 -0.0321335000 _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 0.0370 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 51699 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.806 _diffrn_reflns_theta_min 2.578 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.190 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (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 colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.275 _exptl_crystal_description block _exptl_crystal_F_000 1816 _exptl_crystal_size_max 0.169 _exptl_crystal_size_mid 0.147 _exptl_crystal_size_min 0.136 _refine_diff_density_max 1.140 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 567 _refine_ls_number_reflns 9329 _refine_ls_number_restraints 50 _refine_ls_restrained_S_all 1.028 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0530 _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^)+(0.0848P)^2^+3.7791P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.1442 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8883 _reflns_number_total 9329 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1330 _cod_database_code 1577313 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C36H65Cl2F3N4O3P3S _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 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. 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 2. Uiso/Uaniso restraints and constraints Cl1A \\sim Cl2A \\sim C35A \\sim Cl1B \\sim Cl2B \\sim C35B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A : within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 2A Cl1B \\sim Cl2B \\sim C35B: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 3A Uanis(F1B) = Uanis(F1A) 3. Rigid body (RIGU) restrains Cl1A, Cl2A, C35A, Cl1B, Cl2B, C35B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(C34B)=1-FVAR(1) Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(C34A)=FVAR(1) Sof(Cl1B)=Sof(Cl2B)=Sof(C35B)=Sof(H35C)=Sof(H35D)=1-FVAR(2) Sof(Cl1A)=Sof(Cl2A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C2(H2), C9(H9), C12(H12), C18(H18), C24(H24), C32(H32) 5.b Secondary CH2 refined with riding coordinates: C35A(H35A,H35B), C35B(H35C,H35D), C13(H13A,H13B), C14(H14A,H14B), C15(H15A, H15B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B) 5.c Idealised Me refined as rotating group: C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C33(H33A,H33B, H33C) ; _shelx_res_file ; TITL jjw1330_a.res in P2(1)/c jjw1330.res created by SHELXL-2018/3 at 13:24:32 on 22-Jan-2021 REM Old TITL jjw1330 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.189, Rweak 0.009, Alpha 0.033 REM 1.129 for 384 systematic absences, Orientation as input REM Formula found by SHELXT: C36 N4 O3 F3 S2 Cl4 CELL 1.54184 17.24 14.5891 17.7842 90 96.179 90 ZERR 4 0.0001 0.0001 0.0002 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl F N O P S UNIT 144 256 8 12 16 12 12 4 SIMU Cl1A > C35B SIMU 0.01 0.01 2 Cl1B Cl2B C35B SIMU 0.01 0.01 3 Cl1B Cl2B C35B RIGU Cl1A > C35B EADP F1B F1A L.S. 20 0 0 PLAN 18 CONF FREE Cl1B H17b BOND list 4 fmap 2 53 TEMP 100 MORE -1 ACTA BOND $H REM REM REM WGHT 0.084800 3.779100 FVAR 0.25421 0.78559 0.96930 PART 1 CL1A 3 0.203094 0.103853 0.683742 31.00000 0.05435 0.05212 = 0.16950 0.00185 0.02726 -0.00399 CL2A 3 0.246433 0.146489 0.533432 31.00000 0.12577 0.04340 = 0.09924 0.01314 -0.05552 -0.01970 C35A 1 0.277292 0.103430 0.623460 31.00000 0.04512 0.03609 = 0.09110 0.00660 -0.01568 0.00453 AFIX 23 H35A 2 0.320687 0.140022 0.646008 31.00000 -1.20000 H35B 2 0.295810 0.041147 0.618622 31.00000 -1.20000 AFIX 0 PART 0 PART 2 CL1B 3 0.162688 0.214978 0.517349 -31.00000 0.04477 0.03908 = 0.04499 -0.00275 -0.00052 -0.00739 CL2B 3 0.263390 0.125769 0.395046 -31.00000 0.04747 0.04273 = 0.04963 -0.00116 0.00105 -0.00349 C35B 1 0.229271 0.109494 0.478209 -31.00000 0.03718 0.03406 = 0.04089 0.00104 0.00171 -0.00407 AFIX 23 H35C 2 0.273334 0.098488 0.515822 -31.00000 -1.20000 H35D 2 0.197804 0.054232 0.474750 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 S1A 8 0.490765 0.663222 0.726167 21.00000 0.02834 0.02291 = 0.03894 -0.00278 -0.00530 0.00204 PART 0 PART 2 S1B 8 0.469370 0.627097 0.767764 -21.00000 0.01744 0.02178 = 0.01479 -0.00195 -0.00858 0.00377 PART 0 PART 1 F1A 4 0.362075 0.588369 0.659996 21.00000 0.02785 0.06623 = 0.04829 -0.01074 -0.01262 -0.00406 PART 0 PART 2 F1B 4 0.372062 0.636114 0.646123 -21.00000 0.02785 0.06623 = 0.04829 -0.01074 -0.01262 -0.00406 PART 0 PART 1 F2A 4 0.407919 0.522841 0.763676 21.00000 0.04460 0.05130 = 0.04872 0.00391 0.00485 -0.01293 PART 0 PART 2 F2B 4 0.485574 0.686068 0.632336 -21.00000 0.05708 0.12240 = 0.05652 0.05971 0.01435 0.00585 PART 0 PART 1 F3A 4 0.464323 0.502830 0.662684 21.00000 0.03949 0.04482 = 0.06674 -0.03126 0.00640 -0.00426 PART 0 PART 2 F3B 4 0.464856 0.540571 0.639350 -21.00000 0.09728 0.07689 = 0.03492 -0.03036 0.00453 0.03993 PART 0 PART 1 O1A 6 0.446780 0.717630 0.771815 21.00000 0.04543 0.03732 = 0.03870 -0.01566 -0.00079 0.01484 PART 0 PART 2 O1B 6 0.436282 0.715526 0.790995 -21.00000 0.05118 0.04651 = 0.02351 -0.01612 0.01431 0.01533 PART 0 PART 1 O2A 6 0.502224 0.701573 0.653601 21.00000 0.04641 0.04642 = 0.05665 0.01882 0.00459 0.00024 PART 0 PART 2 O2B 6 0.423639 0.552719 0.792009 -21.00000 0.02747 0.05220 = 0.02697 0.01251 0.00047 -0.00522 PART 0 O3 6 0.558131 0.620608 0.768819 11.00000 0.02995 0.03061 = 0.06771 -0.00497 -0.01918 0.00255 PART 1 C34A 1 0.427844 0.565090 0.702340 21.00000 0.02803 0.03625 = 0.03326 -0.00795 0.00178 -0.00327 PART 0 PART 2 C34B 1 0.448264 0.619823 0.665884 -21.00000 0.01679 0.04881 = 0.02907 -0.00883 -0.00197 0.00241 PART 0 P1 7 0.226069 0.628748 0.472677 11.00000 0.02317 0.01883 = 0.02509 -0.00044 0.00249 0.00014 P2 7 0.160990 0.519601 0.518697 11.00000 0.01936 0.01826 = 0.02164 0.00018 -0.00085 0.00123 P3 7 0.173038 0.734239 0.535401 11.00000 0.02117 0.01852 = 0.02059 -0.00059 -0.00030 0.00004 N1 5 0.236756 0.412436 0.637050 11.00000 0.03692 0.02290 = 0.02365 0.00146 -0.00022 0.00760 N2 5 0.301909 0.407510 0.538807 11.00000 0.02384 0.02208 = 0.02446 -0.00093 -0.00318 0.00522 N3 5 0.259908 0.820066 0.659853 11.00000 0.02688 0.02061 = 0.02193 -0.00187 -0.00122 0.00082 N4 5 0.320849 0.834384 0.559735 11.00000 0.02373 0.02098 = 0.02541 -0.00197 -0.00059 -0.00286 C1 1 0.237197 0.442081 0.564780 11.00000 0.02661 0.01862 = 0.02274 0.00034 -0.00171 0.00247 C2 1 0.172538 0.433516 0.684042 11.00000 0.04831 0.03267 = 0.02787 0.00458 0.01005 0.01058 AFIX 13 H2 2 0.138840 0.477946 0.654965 11.00000 -1.20000 AFIX 0 C3 1 0.201370 0.480684 0.757094 11.00000 0.06659 0.06623 = 0.04929 -0.02237 0.01077 0.01051 AFIX 137 H3A 2 0.158086 0.507937 0.778537 11.00000 -1.50000 H3B 2 0.238155 0.527491 0.747417 11.00000 -1.50000 H3C 2 0.226242 0.436681 0.791881 11.00000 -1.50000 AFIX 0 C4 1 0.122141 0.350870 0.694045 11.00000 0.06028 0.04862 = 0.05769 0.00609 0.02274 0.00751 AFIX 137 H4A 2 0.152818 0.304191 0.721191 11.00000 -1.50000 H4B 2 0.101771 0.327802 0.645332 11.00000 -1.50000 H4C 2 0.079747 0.368001 0.721979 11.00000 -1.50000 AFIX 0 C5 1 0.302687 0.359822 0.657193 11.00000 0.04393 0.02526 = 0.02755 0.00121 -0.00627 0.01267 C6 1 0.322794 0.317710 0.734303 11.00000 0.06588 0.04499 = 0.03264 0.00616 -0.00432 0.02519 AFIX 137 H6A 2 0.364595 0.274600 0.732319 11.00000 -1.50000 H6B 2 0.277868 0.286727 0.749444 11.00000 -1.50000 H6C 2 0.338715 0.365005 0.770216 11.00000 -1.50000 AFIX 0 C7 1 0.343303 0.356373 0.595950 11.00000 0.03278 0.02521 = 0.03209 -0.00175 -0.00817 0.01022 C8 1 0.418187 0.307879 0.588505 11.00000 0.03895 0.03799 = 0.04458 -0.00291 -0.00688 0.01896 AFIX 137 H8A 2 0.412790 0.270902 0.543594 11.00000 -1.50000 H8B 2 0.431048 0.269434 0.631867 11.00000 -1.50000 H8C 2 0.458954 0.352065 0.585259 11.00000 -1.50000 AFIX 0 C9 1 0.324062 0.426076 0.461716 11.00000 0.02174 0.02959 = 0.02901 -0.00023 0.00180 0.00246 AFIX 13 H9 2 0.284816 0.468555 0.437832 11.00000 -1.20000 AFIX 0 C10 1 0.401870 0.475226 0.464245 11.00000 0.02318 0.04549 = 0.04883 0.00494 -0.00037 -0.00297 AFIX 137 H10A 2 0.402540 0.525983 0.498662 11.00000 -1.50000 H10B 2 0.409113 0.497306 0.414631 11.00000 -1.50000 H10C 2 0.443183 0.433482 0.481042 11.00000 -1.50000 AFIX 0 C11 1 0.319388 0.340337 0.412850 11.00000 0.03537 0.03803 = 0.03614 -0.00782 0.00587 0.00644 AFIX 137 H11A 2 0.358691 0.297546 0.432664 11.00000 -1.50000 H11B 2 0.327729 0.356417 0.361998 11.00000 -1.50000 H11C 2 0.268794 0.312905 0.413033 11.00000 -1.50000 AFIX 0 C12 1 0.125076 0.444252 0.436956 11.00000 0.02095 0.02073 = 0.02390 -0.00256 -0.00047 -0.00067 AFIX 13 H12 2 0.167511 0.435050 0.405232 11.00000 -1.20000 AFIX 0 C13 1 0.057282 0.492137 0.390014 11.00000 0.02066 0.03073 = 0.02588 -0.00425 -0.00302 0.00002 AFIX 23 H13A 2 0.015463 0.503219 0.421257 11.00000 -1.20000 H13B 2 0.074634 0.550869 0.372487 11.00000 -1.20000 AFIX 0 C14 1 0.026979 0.433036 0.322046 11.00000 0.02729 0.03845 = 0.02753 -0.00540 -0.00448 -0.00121 AFIX 23 H14A 2 -0.017020 0.463388 0.293859 11.00000 -1.20000 H14B 2 0.067665 0.426077 0.288812 11.00000 -1.20000 AFIX 0 C15 1 0.001836 0.338878 0.347261 11.00000 0.03591 0.04542 = 0.03093 -0.00952 -0.00002 -0.01758 AFIX 23 H15A 2 -0.042806 0.345470 0.375687 11.00000 -1.20000 H15B 2 -0.013946 0.301613 0.303081 11.00000 -1.20000 AFIX 0 C16 1 0.067499 0.290839 0.396139 11.00000 0.05167 0.02704 = 0.03509 -0.00552 0.00254 -0.01190 AFIX 23 H16A 2 0.109578 0.277104 0.365841 11.00000 -1.20000 H16B 2 0.048448 0.233377 0.414541 11.00000 -1.20000 AFIX 0 C17 1 0.098574 0.350859 0.463482 11.00000 0.04121 0.02381 = 0.02962 -0.00095 -0.00148 -0.00694 AFIX 23 H17A 2 0.057948 0.359370 0.496568 11.00000 -1.20000 H17B 2 0.142143 0.320220 0.492110 11.00000 -1.20000 AFIX 0 C18 1 0.137198 0.823303 0.464177 11.00000 0.02316 0.01939 = 0.02371 0.00008 0.00147 0.00313 AFIX 13 H18 2 0.176825 0.832588 0.429325 11.00000 -1.20000 AFIX 0 C19 1 0.062696 0.786413 0.419413 11.00000 0.02333 0.02588 = 0.02673 0.00266 -0.00171 0.00279 AFIX 23 H19A 2 0.073851 0.728521 0.396001 11.00000 -1.20000 H19B 2 0.023400 0.775572 0.453542 11.00000 -1.20000 AFIX 0 C20 1 0.031431 0.855008 0.358240 11.00000 0.02613 0.03457 = 0.02627 0.00564 -0.00143 0.00673 AFIX 23 H20A 2 0.068700 0.860977 0.321376 11.00000 -1.20000 H20B 2 -0.017007 0.831940 0.332268 11.00000 -1.20000 AFIX 0 C21 1 0.017126 0.948744 0.391678 11.00000 0.03906 0.03646 = 0.03106 0.00797 0.00333 0.01630 AFIX 23 H21A 2 -0.025629 0.944506 0.422782 11.00000 -1.20000 H21B 2 0.002158 0.991684 0.351053 11.00000 -1.20000 AFIX 0 C22 1 0.089550 0.984502 0.439495 11.00000 0.05117 0.02395 = 0.02929 0.00454 0.00816 0.01235 AFIX 23 H22A 2 0.076990 1.041497 0.463529 11.00000 -1.20000 H22B 2 0.129997 0.997141 0.407002 11.00000 -1.20000 AFIX 0 C23 1 0.120112 0.915371 0.500183 11.00000 0.03521 0.02172 = 0.02558 0.00002 0.00200 0.00573 AFIX 23 H23A 2 0.081625 0.906836 0.535538 11.00000 -1.20000 H23B 2 0.167422 0.938850 0.528033 11.00000 -1.20000 AFIX 0 C24 1 0.338502 0.826168 0.479803 11.00000 0.02671 0.03048 = 0.02649 -0.00089 0.00328 -0.00342 AFIX 13 H24 2 0.297257 0.787959 0.453729 11.00000 -1.20000 AFIX 0 C25 1 0.414780 0.776083 0.474186 11.00000 0.02899 0.04753 = 0.03963 -0.00561 0.00626 0.00139 AFIX 137 H25A 2 0.420829 0.764536 0.421995 11.00000 -1.50000 H25B 2 0.414382 0.718932 0.500898 11.00000 -1.50000 H25C 2 0.457397 0.813087 0.496111 11.00000 -1.50000 AFIX 0 C26 1 0.333713 0.918664 0.440135 11.00000 0.04287 0.03676 = 0.03508 0.00581 0.00327 -0.01031 AFIX 137 H26A 2 0.375259 0.957332 0.461917 11.00000 -1.50000 H26B 2 0.284462 0.946890 0.446161 11.00000 -1.50000 H26C 2 0.338395 0.910156 0.387287 11.00000 -1.50000 AFIX 0 C27 1 0.365431 0.878966 0.618705 11.00000 0.02660 0.02263 = 0.03012 -0.00282 -0.00361 -0.00182 C28 1 0.442816 0.923239 0.614020 11.00000 0.03239 0.03590 = 0.04204 -0.00500 -0.00226 -0.01045 AFIX 137 H28A 2 0.453230 0.965879 0.654976 11.00000 -1.50000 H28B 2 0.442214 0.955169 0.566761 11.00000 -1.50000 H28C 2 0.482777 0.877143 0.617308 11.00000 -1.50000 AFIX 0 C29 1 0.326584 0.871006 0.681100 11.00000 0.02974 0.01814 = 0.02547 -0.00375 -0.00470 0.00091 C30 1 0.349851 0.908275 0.758727 11.00000 0.03887 0.02588 = 0.02851 -0.00613 -0.00743 -0.00151 AFIX 137 H30A 2 0.374721 0.860908 0.790124 11.00000 -1.50000 H30B 2 0.304300 0.929405 0.780169 11.00000 -1.50000 H30C 2 0.385446 0.958401 0.755645 11.00000 -1.50000 AFIX 0 C31 1 0.146088 0.862274 0.727678 11.00000 0.03553 0.03946 = 0.03930 -0.00166 0.00723 0.00773 AFIX 137 H31A 2 0.174458 0.909679 0.756212 11.00000 -1.50000 H31B 2 0.107226 0.837403 0.756712 11.00000 -1.50000 H31C 2 0.121228 0.887431 0.681336 11.00000 -1.50000 AFIX 0 C32 1 0.201788 0.787128 0.709993 11.00000 0.03186 0.03017 = 0.02566 -0.00143 0.00419 0.00132 AFIX 13 H32 2 0.170084 0.740940 0.680853 11.00000 -1.20000 AFIX 0 C33 1 0.240902 0.737923 0.779400 11.00000 0.04468 0.03529 = 0.03018 0.00183 0.00570 -0.00032 AFIX 137 H33A 2 0.282326 0.699963 0.765006 11.00000 -1.50000 H33B 2 0.203226 0.700486 0.801008 11.00000 -1.50000 H33C 2 0.261835 0.782271 0.815984 11.00000 -1.50000 AFIX 0 C36 1 0.256337 0.798702 0.585215 11.00000 0.02513 0.01998 = 0.02161 -0.00111 -0.00055 0.00152 HKLF 4 REM jjw1330_a.res in P2(1)/c REM wR2 = 0.1442, GooF = S = 1.030, Restrained GooF = 1.028 for all data REM R1 = 0.0530 for 8883 Fo > 4sig(Fo) and 0.0546 for all 9329 data REM 567 parameters refined using 50 restraints END WGHT 0.0848 3.7792 REM Highest difference peak 1.140, deepest hole -0.727, 1-sigma level 0.069 Q1 1 0.1762 1.0017 0.5372 11.00000 0.05 1.14 Q2 1 0.1874 0.1343 0.6425 11.00000 0.05 0.93 Q3 1 0.3986 0.1210 0.5064 11.00000 0.05 0.79 Q4 1 0.1988 0.5240 0.7204 11.00000 0.05 0.76 Q5 1 0.5135 0.5749 0.7772 11.00000 0.05 0.74 Q6 1 0.2858 0.1180 0.5394 11.00000 0.05 0.74 Q7 1 0.2152 0.7042 0.7345 11.00000 0.05 0.58 Q8 1 0.2362 0.5876 0.5378 11.00000 0.05 0.56 Q9 1 0.2046 0.6371 0.6854 11.00000 0.05 0.56 Q10 1 0.1993 0.1597 0.5838 11.00000 0.05 0.54 Q11 1 0.3625 0.3407 0.7298 11.00000 0.05 0.47 Q12 1 0.4829 0.5972 0.7233 11.00000 0.05 0.47 Q13 1 0.0586 0.9525 0.4136 11.00000 0.05 0.41 Q14 1 0.3365 0.3802 0.6423 11.00000 0.05 0.39 Q15 1 0.5445 0.6414 0.7617 11.00000 0.05 0.37 Q16 1 0.3200 0.9009 0.5614 11.00000 0.05 0.36 Q17 1 0.1065 0.3953 0.4557 11.00000 0.05 0.35 Q18 1 0.0140 0.4009 0.3508 11.00000 0.05 0.34 ; _shelx_res_checksum 30023 _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 1.596 _oxdiff_exptl_absorpt_empirical_full_min 0.811 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 Cl1A Cl 0.20309(5) 0.10385(7) 0.68374(9) 0.0909(4) Uani 0.9693(18) 1 d . U P A 1 Cl2A Cl 0.24643(8) 0.14649(6) 0.53343(7) 0.0944(4) Uani 0.9693(18) 1 d . U P A 1 C35A C 0.27729(18) 0.1034(2) 0.6235(2) 0.0591(8) Uani 0.9693(18) 1 d . U P A 1 H35A H 0.320687 0.140022 0.646008 0.071 Uiso 0.9693(18) 1 calc R U P A 1 H35B H 0.295810 0.041147 0.618622 0.071 Uiso 0.9693(18) 1 calc R U P A 1 Cl1B Cl 0.1627(12) 0.2150(14) 0.5173(11) 0.043(5) Uani 0.0307(18) 1 d . U P A 2 Cl2B Cl 0.2634(13) 0.1258(14) 0.3950(13) 0.047(5) Uani 0.0307(18) 1 d . U P A 2 C35B C 0.229(5) 0.109(5) 0.478(4) 0.038(6) Uani 0.0307(18) 1 d . U P A 2 H35C H 0.273334 0.098488 0.515822 0.045 Uiso 0.0307(18) 1 calc R U P A 2 H35D H 0.197804 0.054232 0.474750 0.045 Uiso 0.0307(18) 1 calc R U P A 2 S1A S 0.49076(4) 0.66322(4) 0.72617(4) 0.0307(2) Uani 0.786(2) 1 d . . P B 1 S1B S 0.46937(11) 0.62710(14) 0.76776(11) 0.0188(7) Uani 0.214(2) 1 d . . P B 2 F1A F 0.36208(11) 0.58837(18) 0.66000(12) 0.0487(5) Uani 0.786(2) 1 d . . P B 1 F1B F 0.3721(5) 0.6361(7) 0.6461(5) 0.0487(5) Uani 0.214(2) 1 d . . P B 2 F2A F 0.40792(15) 0.52284(18) 0.76368(15) 0.0482(6) Uani 0.786(2) 1 d . . P B 1 F2B F 0.4856(12) 0.6861(17) 0.6323(11) 0.078(6) Uani 0.214(2) 1 d . . P B 2 F3A F 0.46432(16) 0.50283(19) 0.66268(19) 0.0503(7) Uani 0.786(2) 1 d . . P B 1 F3B F 0.4649(9) 0.5406(9) 0.6393(6) 0.070(4) Uani 0.214(2) 1 d . . P B 2 O1A O 0.4468(4) 0.7176(6) 0.7718(3) 0.0409(11) Uani 0.786(2) 1 d . . P B 1 O1B O 0.4363(19) 0.716(2) 0.7910(12) 0.040(4) Uani 0.214(2) 1 d . . P B 2 O2A O 0.5022(4) 0.7016(4) 0.6536(3) 0.0499(11) Uani 0.786(2) 1 d . . P B 1 O2B O 0.4236(5) 0.5527(8) 0.7920(5) 0.036(2) Uani 0.214(2) 1 d . . P B 2 O3 O 0.55813(10) 0.62061(11) 0.76882(12) 0.0445(4) Uani 1 1 d . . . . . C34A C 0.42784(16) 0.5651(2) 0.70234(16) 0.0326(6) Uani 0.786(2) 1 d . . P B 1 C34B C 0.4483(5) 0.6198(8) 0.6659(6) 0.032(2) Uani 0.214(2) 1 d . . P B 2 P1 P 0.22607(3) 0.62875(3) 0.47268(3) 0.02238(12) Uani 1 1 d . . . . . P2 P 0.16099(3) 0.51960(3) 0.51870(3) 0.01997(12) Uani 1 1 d . . . . . P3 P 0.17304(3) 0.73424(3) 0.53540(3) 0.02028(12) Uani 1 1 d . . . . . N1 N 0.23676(11) 0.41244(12) 0.63705(9) 0.0281(4) Uani 1 1 d . . . . . N2 N 0.30191(9) 0.40751(11) 0.53881(9) 0.0239(3) Uani 1 1 d . . . . . N3 N 0.25991(9) 0.82007(11) 0.65985(9) 0.0234(3) Uani 1 1 d . . . . . N4 N 0.32085(9) 0.83438(11) 0.55974(9) 0.0236(3) Uani 1 1 d . . . . . C1 C 0.23720(11) 0.44208(12) 0.56478(10) 0.0230(4) Uani 1 1 d . . . . . C2 C 0.17254(15) 0.43352(16) 0.68404(12) 0.0359(5) Uani 1 1 d . . . . . H2 H 0.138840 0.477946 0.654965 0.043 Uiso 1 1 calc R U . . . C3 C 0.2014(2) 0.4807(2) 0.75709(18) 0.0604(8) Uani 1 1 d . . . . . H3A H 0.158086 0.507937 0.778537 0.091 Uiso 1 1 calc R U . . . H3B H 0.238155 0.527491 0.747417 0.091 Uiso 1 1 calc R U . . . H3C H 0.226242 0.436681 0.791881 0.091 Uiso 1 1 calc R U . . . C4 C 0.12214(19) 0.3509(2) 0.69404(18) 0.0543(7) Uani 1 1 d . . . . . H4A H 0.152818 0.304191 0.721191 0.082 Uiso 1 1 calc R U . . . H4B H 0.101771 0.327802 0.645332 0.082 Uiso 1 1 calc R U . . . H4C H 0.079747 0.368001 0.721979 0.082 Uiso 1 1 calc R U . . . C5 C 0.30269(14) 0.35982(15) 0.65719(12) 0.0330(5) Uani 1 1 d . . . . . C6 C 0.32279(18) 0.31771(19) 0.73430(14) 0.0485(6) Uani 1 1 d . . . . . H6A H 0.364595 0.274600 0.732319 0.073 Uiso 1 1 calc R U . . . H6B H 0.277868 0.286727 0.749444 0.073 Uiso 1 1 calc R U . . . H6C H 0.338715 0.365005 0.770216 0.073 Uiso 1 1 calc R U . . . C7 C 0.34330(13) 0.35637(14) 0.59595(12) 0.0309(4) Uani 1 1 d . . . . . C8 C 0.41819(14) 0.30788(18) 0.58851(15) 0.0413(5) Uani 1 1 d . . . . . H8A H 0.412790 0.270902 0.543594 0.062 Uiso 1 1 calc R U . . . H8B H 0.431048 0.269434 0.631867 0.062 Uiso 1 1 calc R U . . . H8C H 0.458954 0.352065 0.585259 0.062 Uiso 1 1 calc R U . . . C9 C 0.32406(11) 0.42608(14) 0.46172(11) 0.0268(4) Uani 1 1 d . . . . . H9 H 0.284816 0.468555 0.437832 0.032 Uiso 1 1 calc R U . . . C10 C 0.40187(12) 0.47523(18) 0.46425(15) 0.0395(5) Uani 1 1 d . . . . . H10A H 0.402540 0.525983 0.498662 0.059 Uiso 1 1 calc R U . . . H10B H 0.409113 0.497306 0.414631 0.059 Uiso 1 1 calc R U . . . H10C H 0.443183 0.433482 0.481042 0.059 Uiso 1 1 calc R U . . . C11 C 0.31939(14) 0.34034(17) 0.41285(13) 0.0364(5) Uani 1 1 d . . . . . H11A H 0.358691 0.297546 0.432664 0.055 Uiso 1 1 calc R U . . . H11B H 0.327729 0.356417 0.361998 0.055 Uiso 1 1 calc R U . . . H11C H 0.268794 0.312905 0.413033 0.055 Uiso 1 1 calc R U . . . C12 C 0.12508(10) 0.44425(13) 0.43696(10) 0.0221(4) Uani 1 1 d . . . . . H12 H 0.167511 0.435050 0.405232 0.026 Uiso 1 1 calc R U . . . C13 C 0.05728(11) 0.49214(14) 0.39001(11) 0.0262(4) Uani 1 1 d . . . . . H13A H 0.015463 0.503219 0.421257 0.031 Uiso 1 1 calc R U . . . H13B H 0.074634 0.550869 0.372487 0.031 Uiso 1 1 calc R U . . . C14 C 0.02698(12) 0.43304(16) 0.32205(12) 0.0316(4) Uani 1 1 d . . . . . H14A H -0.017020 0.463388 0.293859 0.038 Uiso 1 1 calc R U . . . H14B H 0.067665 0.426077 0.288812 0.038 Uiso 1 1 calc R U . . . C15 C 0.00184(14) 0.33888(17) 0.34726(13) 0.0377(5) Uani 1 1 d . . . . . H15A H -0.042806 0.345470 0.375687 0.045 Uiso 1 1 calc R U . . . H15B H -0.013946 0.301613 0.303081 0.045 Uiso 1 1 calc R U . . . C16 C 0.06750(15) 0.29084(16) 0.39614(13) 0.0381(5) Uani 1 1 d . . . . . H16A H 0.109578 0.277104 0.365841 0.046 Uiso 1 1 calc R U . . . H16B H 0.048448 0.233377 0.414541 0.046 Uiso 1 1 calc R U . . . C17 C 0.09857(14) 0.35086(14) 0.46348(12) 0.0319(4) Uani 1 1 d . . . . . H17A H 0.057948 0.359370 0.496568 0.038 Uiso 1 1 calc R U . . . H17B H 0.142143 0.320220 0.492110 0.038 Uiso 1 1 calc R U . . . C18 C 0.13720(11) 0.82330(12) 0.46418(10) 0.0222(4) Uani 1 1 d . . . . . H18 H 0.176825 0.832588 0.429325 0.027 Uiso 1 1 calc R U . . . C19 C 0.06270(11) 0.78641(14) 0.41941(11) 0.0256(4) Uani 1 1 d . . . . . H19A H 0.073851 0.728521 0.396001 0.031 Uiso 1 1 calc R U . . . H19B H 0.023400 0.775572 0.453542 0.031 Uiso 1 1 calc R U . . . C20 C 0.03143(12) 0.85501(15) 0.35824(12) 0.0293(4) Uani 1 1 d . . . . . H20A H 0.068700 0.860977 0.321376 0.035 Uiso 1 1 calc R U . . . H20B H -0.017007 0.831940 0.332268 0.035 Uiso 1 1 calc R U . . . C21 C 0.01713(13) 0.94874(16) 0.39168(12) 0.0356(5) Uani 1 1 d . . . . . H21A H -0.025629 0.944506 0.422782 0.043 Uiso 1 1 calc R U . . . H21B H 0.002158 0.991684 0.351053 0.043 Uiso 1 1 calc R U . . . C22 C 0.08955(14) 0.98450(14) 0.43950(12) 0.0345(5) Uani 1 1 d . . . . . H22A H 0.076990 1.041497 0.463529 0.041 Uiso 1 1 calc R U . . . H22B H 0.129997 0.997141 0.407002 0.041 Uiso 1 1 calc R U . . . C23 C 0.12011(12) 0.91537(13) 0.50018(11) 0.0276(4) Uani 1 1 d . . . . . H23A H 0.081625 0.906836 0.535538 0.033 Uiso 1 1 calc R U . . . H23B H 0.167422 0.938850 0.528033 0.033 Uiso 1 1 calc R U . . . C24 C 0.33850(12) 0.82617(15) 0.47980(11) 0.0279(4) Uani 1 1 d . . . . . H24 H 0.297257 0.787959 0.453729 0.033 Uiso 1 1 calc R U . . . C25 C 0.41478(13) 0.77608(18) 0.47419(14) 0.0385(5) Uani 1 1 d . . . . . H25A H 0.420829 0.764536 0.421995 0.058 Uiso 1 1 calc R U . . . H25B H 0.414382 0.718932 0.500898 0.058 Uiso 1 1 calc R U . . . H25C H 0.457397 0.813087 0.496111 0.058 Uiso 1 1 calc R U . . . C26 C 0.33371(15) 0.91866(17) 0.44014(13) 0.0383(5) Uani 1 1 d . . . . . H26A H 0.375259 0.957332 0.461917 0.057 Uiso 1 1 calc R U . . . H26B H 0.284462 0.946890 0.446161 0.057 Uiso 1 1 calc R U . . . H26C H 0.338395 0.910156 0.387287 0.057 Uiso 1 1 calc R U . . . C27 C 0.36543(12) 0.87897(13) 0.61871(12) 0.0269(4) Uani 1 1 d . . . . . C28 C 0.44282(13) 0.92324(17) 0.61402(14) 0.0372(5) Uani 1 1 d . . . . . H28A H 0.453230 0.965879 0.654976 0.056 Uiso 1 1 calc R U . . . H28B H 0.442214 0.955169 0.566761 0.056 Uiso 1 1 calc R U . . . H28C H 0.482777 0.877143 0.617308 0.056 Uiso 1 1 calc R U . . . C29 C 0.32658(12) 0.87101(12) 0.68110(11) 0.0250(4) Uani 1 1 d . . . . . C30 C 0.34985(13) 0.90828(14) 0.75873(12) 0.0319(4) Uani 1 1 d . . . . . H30A H 0.374721 0.860908 0.790124 0.048 Uiso 1 1 calc R U . . . H30B H 0.304300 0.929405 0.780169 0.048 Uiso 1 1 calc R U . . . H30C H 0.385446 0.958401 0.755645 0.048 Uiso 1 1 calc R U . . . C31 C 0.14609(14) 0.86227(17) 0.72768(14) 0.0379(5) Uani 1 1 d . . . . . H31A H 0.174458 0.909679 0.756212 0.057 Uiso 1 1 calc R U . . . H31B H 0.107226 0.837403 0.756712 0.057 Uiso 1 1 calc R U . . . H31C H 0.121228 0.887431 0.681336 0.057 Uiso 1 1 calc R U . . . C32 C 0.20179(12) 0.78713(15) 0.70999(11) 0.0292(4) Uani 1 1 d . . . . . H32 H 0.170084 0.740940 0.680853 0.035 Uiso 1 1 calc R U . . . C33 C 0.24090(14) 0.73792(16) 0.77940(13) 0.0366(5) Uani 1 1 d . . . . . H33A H 0.282326 0.699963 0.765006 0.055 Uiso 1 1 calc R U . . . H33B H 0.203226 0.700486 0.801008 0.055 Uiso 1 1 calc R U . . . H33C H 0.261835 0.782271 0.815984 0.055 Uiso 1 1 calc R U . . . C36 C 0.25634(11) 0.79870(12) 0.58521(10) 0.0225(4) 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 Cl1A 0.0543(5) 0.0521(5) 0.1695(12) 0.0019(6) 0.0273(6) -0.0040(4) Cl2A 0.1258(9) 0.0434(4) 0.0992(8) 0.0131(4) -0.0555(7) -0.0197(5) C35A 0.0451(15) 0.0361(14) 0.091(2) 0.0066(15) -0.0157(15) 0.0045(12) Cl1B 0.045(9) 0.039(9) 0.045(9) -0.003(7) -0.001(7) -0.007(7) Cl2B 0.047(9) 0.043(9) 0.050(10) -0.001(7) 0.001(7) -0.003(7) C35B 0.037(10) 0.034(10) 0.041(10) 0.001(8) 0.002(9) -0.004(9) S1A 0.0283(3) 0.0229(3) 0.0389(4) -0.0028(3) -0.0053(3) 0.0020(2) S1B 0.0174(10) 0.0218(11) 0.0148(11) -0.0019(8) -0.0086(7) 0.0038(7) F1A 0.0279(8) 0.0662(15) 0.0483(11) -0.0107(11) -0.0126(7) -0.0041(10) F1B 0.0279(8) 0.0662(15) 0.0483(11) -0.0107(11) -0.0126(7) -0.0041(10) F2A 0.0446(13) 0.0513(14) 0.0487(14) 0.0039(10) 0.0049(11) -0.0129(10) F2B 0.057(10) 0.122(16) 0.057(10) 0.060(10) 0.014(7) 0.006(8) F3A 0.0395(11) 0.0448(15) 0.067(2) -0.0313(12) 0.0064(12) -0.0043(11) F3B 0.097(8) 0.077(9) 0.035(5) -0.030(5) 0.005(5) 0.040(7) O1A 0.045(2) 0.0373(15) 0.039(3) -0.016(2) -0.001(2) 0.0148(16) O1B 0.051(8) 0.047(6) 0.024(8) -0.016(6) 0.014(5) 0.015(5) O2A 0.046(2) 0.0464(16) 0.057(3) 0.0188(17) 0.0046(18) 0.0002(15) O2B 0.027(4) 0.052(6) 0.027(4) 0.013(4) 0.000(3) -0.005(4) O3 0.0300(8) 0.0306(8) 0.0677(12) -0.0050(8) -0.0192(8) 0.0025(6) C34A 0.0280(13) 0.0363(15) 0.0333(14) -0.0080(12) 0.0018(11) -0.0033(11) C34B 0.017(4) 0.049(6) 0.029(5) -0.009(4) -0.002(3) 0.002(4) P1 0.0232(2) 0.0188(2) 0.0251(2) -0.00044(16) 0.00249(17) 0.00014(16) P2 0.0194(2) 0.0183(2) 0.0216(2) 0.00018(16) -0.00085(16) 0.00123(15) P3 0.0212(2) 0.0185(2) 0.0206(2) -0.00059(16) -0.00030(16) 0.00004(16) N1 0.0369(9) 0.0229(8) 0.0237(8) 0.0015(6) -0.0002(7) 0.0076(7) N2 0.0238(7) 0.0221(8) 0.0245(8) -0.0009(6) -0.0032(6) 0.0052(6) N3 0.0269(8) 0.0206(7) 0.0219(7) -0.0019(6) -0.0012(6) 0.0008(6) N4 0.0237(7) 0.0210(7) 0.0254(8) -0.0020(6) -0.0006(6) -0.0029(6) C1 0.0266(9) 0.0186(8) 0.0227(8) 0.0003(7) -0.0017(7) 0.0025(7) C2 0.0483(13) 0.0327(11) 0.0279(10) 0.0046(8) 0.0100(9) 0.0106(9) C3 0.0666(19) 0.066(2) 0.0493(16) -0.0224(14) 0.0108(14) 0.0105(15) C4 0.0603(17) 0.0486(15) 0.0577(17) 0.0061(13) 0.0227(14) 0.0075(13) C5 0.0439(12) 0.0253(10) 0.0275(10) 0.0012(8) -0.0063(9) 0.0127(9) C6 0.0659(17) 0.0450(14) 0.0326(12) 0.0062(10) -0.0043(11) 0.0252(13) C7 0.0328(10) 0.0252(9) 0.0321(10) -0.0018(8) -0.0082(8) 0.0102(8) C8 0.0390(12) 0.0380(12) 0.0446(13) -0.0029(10) -0.0069(10) 0.0190(10) C9 0.0217(9) 0.0296(10) 0.0290(10) -0.0002(8) 0.0018(7) 0.0025(7) C10 0.0232(10) 0.0455(13) 0.0488(13) 0.0049(10) -0.0004(9) -0.0030(9) C11 0.0354(11) 0.0380(12) 0.0361(11) -0.0078(9) 0.0059(9) 0.0064(9) C12 0.0210(8) 0.0207(8) 0.0239(8) -0.0026(7) -0.0005(7) -0.0007(7) C13 0.0207(8) 0.0307(10) 0.0259(9) -0.0043(8) -0.0030(7) 0.0000(7) C14 0.0273(9) 0.0384(11) 0.0275(10) -0.0054(8) -0.0045(8) -0.0012(8) C15 0.0359(11) 0.0454(13) 0.0309(11) -0.0095(9) 0.0000(9) -0.0176(10) C16 0.0517(13) 0.0270(10) 0.0351(11) -0.0055(9) 0.0025(10) -0.0119(9) C17 0.0412(11) 0.0238(9) 0.0296(10) -0.0009(8) -0.0015(8) -0.0069(8) C18 0.0232(8) 0.0194(8) 0.0237(8) 0.0001(7) 0.0015(7) 0.0031(7) C19 0.0233(9) 0.0259(9) 0.0267(9) 0.0027(7) -0.0017(7) 0.0028(7) C20 0.0261(9) 0.0346(10) 0.0263(9) 0.0056(8) -0.0014(7) 0.0067(8) C21 0.0391(11) 0.0365(12) 0.0311(10) 0.0080(9) 0.0033(9) 0.0163(9) C22 0.0512(13) 0.0239(10) 0.0293(10) 0.0045(8) 0.0082(9) 0.0123(9) C23 0.0352(10) 0.0217(9) 0.0256(9) 0.0000(7) 0.0020(8) 0.0057(8) C24 0.0267(9) 0.0305(10) 0.0265(9) -0.0009(8) 0.0033(7) -0.0034(8) C25 0.0290(10) 0.0475(13) 0.0396(12) -0.0056(10) 0.0063(9) 0.0014(9) C26 0.0429(12) 0.0368(12) 0.0351(11) 0.0058(9) 0.0033(9) -0.0103(10) C27 0.0266(9) 0.0226(9) 0.0301(10) -0.0028(7) -0.0036(8) -0.0018(7) C28 0.0324(11) 0.0359(11) 0.0420(12) -0.0050(9) -0.0023(9) -0.0104(9) C29 0.0297(10) 0.0181(8) 0.0255(9) -0.0037(7) -0.0047(7) 0.0009(7) C30 0.0389(11) 0.0259(10) 0.0285(10) -0.0061(8) -0.0074(8) -0.0015(8) C31 0.0355(11) 0.0395(12) 0.0393(12) -0.0017(9) 0.0072(9) 0.0077(9) C32 0.0319(10) 0.0302(10) 0.0257(9) -0.0014(8) 0.0042(8) 0.0013(8) C33 0.0447(12) 0.0353(11) 0.0302(11) 0.0018(9) 0.0057(9) -0.0003(9) C36 0.0251(9) 0.0200(8) 0.0216(8) -0.0011(7) -0.0006(7) 0.0015(7) 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 0 -1 -1 0.0396 5 -4 0 0.0650 5 -1 1 0.0728 2 5 2 0.0819 -1 1 0 0.0909 -5 1 -1 0.0930 -3 1 5 0.0702 -5 -1 2 0.0828 2 -2 -5 0.0607 5 2 -1 0.0781 -2 -3 -5 0.0590 -2 5 -4 0.0684 -5 1 -4 0.0726 3 5 -1 0.0767 1 2 -5 0.0595 5 4 -1 0.0733 0 -5 4 0.0808 -2 -3 5 0.0774 2 -5 3 0.0706 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 Cl1A C35A H35A 109.0 . . ? Cl1A C35A H35B 109.0 . . ? Cl2A C35A Cl1A 112.83(17) . . ? Cl2A C35A H35A 109.0 . . ? Cl2A C35A H35B 109.0 . . ? H35A C35A H35B 107.8 . . ? Cl1B C35B H35C 108.1 . . ? Cl1B C35B H35D 108.1 . . ? Cl2B C35B Cl1B 117(4) . . ? Cl2B C35B H35C 108.1 . . ? Cl2B C35B H35D 108.1 . . ? H35C C35B H35D 107.3 . . ? O1A S1A O2A 115.5(4) . . ? O1A S1A O3 112.8(3) . . ? O1A S1A C34A 103.4(4) . . ? O2A S1A O3 117.0(3) . . ? O2A S1A C34A 103.5(2) . . ? O3 S1A C34A 101.98(12) . . ? O1B S1B O3 117.6(13) . . ? O1B S1B C34B 106.7(11) . . ? O2B S1B O1B 109.5(12) . . ? O2B S1B O3 122.0(4) . . ? O2B S1B C34B 101.4(5) . . ? O3 S1B C34B 95.8(3) . . ? F1A C34A S1A 112.3(2) . . ? F1A C34A F3A 107.0(2) . . ? F2A C34A S1A 112.0(2) . . ? F2A C34A F1A 107.6(3) . . ? F2A C34A F3A 107.1(3) . . ? F3A C34A S1A 110.6(2) . . ? F1B C34B S1B 109.7(7) . . ? F2B C34B S1B 110.5(10) . . ? F2B C34B F1B 105.0(13) . . ? F3B C34B S1B 112.9(9) . . ? F3B C34B F1B 108.1(10) . . ? F3B C34B F2B 110.4(15) . . ? P2 P1 P3 93.65(2) . . ? C1 P2 P1 104.17(6) . . ? C1 P2 C12 98.29(8) . . ? C12 P2 P1 106.28(6) . . ? C18 P3 P1 105.79(6) . . ? C36 P3 P1 104.96(6) . . ? C36 P3 C18 98.80(8) . . ? C1 N1 C2 123.09(17) . . ? C1 N1 C5 109.46(17) . . ? C5 N1 C2 127.42(18) . . ? C1 N2 C7 109.12(17) . . ? C1 N2 C9 123.43(15) . . ? C7 N2 C9 127.41(17) . . ? C29 N3 C32 126.91(16) . . ? C36 N3 C29 109.77(16) . . ? C36 N3 C32 123.22(16) . . ? C27 N4 C24 127.08(17) . . ? C36 N4 C24 123.33(16) . . ? C36 N4 C27 109.58(16) . . ? N1 C1 P2 122.45(14) . . ? N2 C1 P2 130.40(14) . . ? N2 C1 N1 107.10(16) . . ? N1 C2 H2 105.9 . . ? N1 C2 C3 112.5(2) . . ? N1 C2 C4 111.9(2) . . ? C3 C2 H2 105.9 . . ? C3 C2 C4 113.9(2) . . ? C4 C2 H2 105.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? 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 . . ? N1 C5 C6 124.2(2) . . ? C7 C5 N1 107.01(18) . . ? C7 C5 C6 128.8(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 124.7(2) . . ? C5 C7 N2 107.29(18) . . ? C5 C7 C8 128.0(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 H9 106.3 . . ? N2 C9 C10 111.88(17) . . ? N2 C9 C11 111.97(17) . . ? C10 C9 H9 106.3 . . ? C10 C9 C11 113.46(18) . . ? C11 C9 H9 106.3 . . ? 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 108.8 . . ? C13 C12 P2 108.94(13) . . ? C13 C12 H12 108.8 . . ? C17 C12 P2 111.62(13) . . ? C17 C12 H12 108.8 . . ? C17 C12 C13 109.84(16) . . ? C12 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C14 C13 C12 110.46(16) . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C15 C14 C13 111.07(18) . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C14 C15 H15A 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C16 C15 C14 111.46(18) . . ? C16 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? C15 C16 C17 111.04(19) . . ? H16A C16 H16B 108.0 . . ? C17 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C12 C17 C16 111.05(17) . . ? C12 C17 H17A 109.4 . . ? C12 C17 H17B 109.4 . . ? C16 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? P3 C18 H18 108.8 . . ? C19 C18 P3 107.73(13) . . ? C19 C18 H18 108.8 . . ? C23 C18 P3 112.98(13) . . ? C23 C18 H18 108.8 . . ? C23 C18 C19 109.69(16) . . ? C18 C19 H19A 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C20 C19 C18 110.50(16) . . ? C20 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C19 C20 H20A 109.3 . . ? C19 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C21 C20 C19 111.64(17) . . ? C21 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C20 C21 H21A 109.3 . . ? C20 C21 H21B 109.3 . . ? C20 C21 C22 111.59(17) . . ? H21A C21 H21B 108.0 . . ? C22 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C21 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C21 C22 C23 111.55(18) . . ? H22A C22 H22B 108.0 . . ? C23 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C22 C23 C18 110.54(16) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? N4 C24 H24 106.5 . . ? N4 C24 C25 111.66(17) . . ? N4 C24 C26 111.39(18) . . ? C25 C24 H24 106.5 . . ? C25 C24 C26 113.64(19) . . ? C26 C24 H24 106.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N4 C27 C28 125.74(19) . . ? C29 C27 N4 107.09(17) . . ? C29 C27 C28 127.12(19) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C30 125.28(19) . . ? C27 C29 N3 106.84(16) . . ? C27 C29 C30 127.87(19) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? N3 C32 C31 111.92(18) . . ? N3 C32 H32 106.1 . . ? N3 C32 C33 111.69(17) . . ? C31 C32 H32 106.1 . . ? C31 C32 C33 114.15(18) . . ? C33 C32 H32 106.1 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C36 P3 122.21(14) . . ? N4 C36 P3 131.08(14) . . ? N4 C36 N3 106.69(16) . . ? 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 Cl1A C35A 1.755(4) . ? Cl2A C35A 1.749(4) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? Cl1B C35B 2.08(8) . ? Cl2B C35B 1.67(8) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? S1A O1A 1.413(6) . ? S1A O2A 1.440(7) . ? S1A O3 1.4564(17) . ? S1A C34A 1.819(3) . ? S1B O1B 1.49(3) . ? S1B O2B 1.435(10) . ? S1B O3 1.531(3) . ? S1B C34B 1.812(10) . ? F1A C34A 1.336(3) . ? F1B C34B 1.344(12) . ? F2A C34A 1.330(4) . ? F2B C34B 1.34(2) . ? F3A C34A 1.347(4) . ? F3B C34B 1.292(16) . ? P1 P2 2.1591(6) . ? P1 P3 2.1606(6) . ? P2 C1 1.8561(19) . ? P2 C12 1.8738(18) . ? P3 C18 1.8725(19) . ? P3 C36 1.8595(19) . ? N1 C1 1.357(2) . ? N1 C2 1.489(3) . ? N1 C5 1.386(3) . ? N2 C1 1.350(2) . ? N2 C7 1.394(2) . ? N2 C9 1.487(3) . ? N3 C29 1.387(2) . ? N3 C32 1.491(3) . ? N3 C36 1.358(2) . ? N4 C24 1.490(2) . ? N4 C27 1.393(2) . ? N4 C36 1.350(2) . ? C2 H2 0.9800 . ? C2 C3 1.506(4) . ? C2 C4 1.508(4) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.509(3) . ? C5 C7 1.358(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.490(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9 0.9800 . ? C9 C10 1.517(3) . ? C9 C11 1.520(3) . ? 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 1.530(2) . ? C12 C17 1.528(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.530(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.522(3) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.522(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.533(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18 0.9800 . ? C18 C19 1.534(3) . ? C18 C23 1.530(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.533(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.522(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.525(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.529(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24 0.9800 . ? C24 C25 1.517(3) . ? C24 C26 1.521(3) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.493(3) . ? C27 C29 1.361(3) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.498(3) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C31 C32 1.513(3) . ? C32 H32 0.9800 . ? C32 C33 1.521(3) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 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 O1A S1A C34A F1A 64.8(4) . . . . ? O1A S1A C34A F2A -56.3(4) . . . . ? O1A S1A C34A F3A -175.7(4) . . . . ? O1B S1B C34B F1B -50.8(15) . . . . ? O1B S1B C34B F2B 64.5(18) . . . . ? O1B S1B C34B F3B -171.4(16) . . . . ? O2A S1A C34A F1A -56.0(3) . . . . ? O2A S1A C34A F2A -177.2(3) . . . . ? O2A S1A C34A F3A 63.5(4) . . . . ? O2B S1B C34B F1B 63.8(9) . . . . ? O2B S1B C34B F2B 179.1(13) . . . . ? O2B S1B C34B F3B -56.9(11) . . . . ? O3 S1A C34A F1A -177.9(2) . . . . ? O3 S1A C34A F2A 60.9(2) . . . . ? O3 S1A C34A F3A -58.4(3) . . . . ? O3 S1B C34B F1B -171.8(8) . . . . ? O3 S1B C34B F2B -56.6(13) . . . . ? O3 S1B C34B F3B 67.5(10) . . . . ? P1 P2 C1 N1 129.36(15) . . . . ? P1 P2 C1 N2 -47.90(19) . . . . ? P1 P2 C12 C13 -74.87(13) . . . . ? P1 P2 C12 C17 163.66(13) . . . . ? P1 P3 C18 C19 75.88(13) . . . . ? P1 P3 C18 C23 -162.79(13) . . . . ? P1 P3 C36 N3 -132.58(14) . . . . ? P1 P3 C36 N4 48.97(19) . . . . ? P2 C12 C13 C14 179.32(14) . . . . ? P2 C12 C17 C16 178.61(16) . . . . ? P3 C18 C19 C20 -178.31(13) . . . . ? P3 C18 C23 C22 -178.84(15) . . . . ? N1 C5 C7 N2 0.3(2) . . . . ? N1 C5 C7 C8 -179.6(2) . . . . ? N4 C27 C29 N3 1.3(2) . . . . ? N4 C27 C29 C30 -179.23(18) . . . . ? C1 P2 C12 C13 177.66(13) . . . . ? C1 P2 C12 C17 56.19(15) . . . . ? C1 N1 C2 C3 -123.5(2) . . . . ? C1 N1 C2 C4 106.8(2) . . . . ? C1 N1 C5 C6 178.2(2) . . . . ? C1 N1 C5 C7 -0.8(2) . . . . ? C1 N2 C7 C5 0.3(2) . . . . ? C1 N2 C7 C8 -179.8(2) . . . . ? C1 N2 C9 C10 118.4(2) . . . . ? C1 N2 C9 C11 -113.0(2) . . . . ? C2 N1 C1 P2 4.6(3) . . . . ? C2 N1 C1 N2 -177.59(18) . . . . ? C2 N1 C5 C6 -3.3(4) . . . . ? C2 N1 C5 C7 177.7(2) . . . . ? C5 N1 C1 P2 -176.82(15) . . . . ? C5 N1 C1 N2 1.0(2) . . . . ? C5 N1 C2 C3 58.1(3) . . . . ? C5 N1 C2 C4 -71.5(3) . . . . ? C6 C5 C7 N2 -178.6(2) . . . . ? C6 C5 C7 C8 1.5(4) . . . . ? C7 N2 C1 P2 176.79(15) . . . . ? C7 N2 C1 N1 -0.8(2) . . . . ? C7 N2 C9 C10 -59.3(3) . . . . ? C7 N2 C9 C11 69.4(2) . . . . ? C9 N2 C1 P2 -1.2(3) . . . . ? C9 N2 C1 N1 -178.83(17) . . . . ? C9 N2 C7 C5 178.23(19) . . . . ? C9 N2 C7 C8 -1.8(3) . . . . ? C12 P2 C1 N1 -121.43(16) . . . . ? C12 P2 C1 N2 61.31(19) . . . . ? C12 C13 C14 C15 57.2(2) . . . . ? C13 C12 C17 C16 57.7(2) . . . . ? C13 C14 C15 C16 -55.4(2) . . . . ? C14 C15 C16 C17 54.6(3) . . . . ? C15 C16 C17 C12 -56.0(3) . . . . ? C17 C12 C13 C14 -58.1(2) . . . . ? C18 P3 C36 N3 118.36(16) . . . . ? C18 P3 C36 N4 -60.09(19) . . . . ? C18 C19 C20 C21 -56.1(2) . . . . ? C19 C18 C23 C22 -58.6(2) . . . . ? C19 C20 C21 C22 53.6(2) . . . . ? C20 C21 C22 C23 -53.9(2) . . . . ? C21 C22 C23 C18 56.6(2) . . . . ? C23 C18 C19 C20 58.3(2) . . . . ? C24 N4 C27 C28 -3.7(3) . . . . ? C24 N4 C27 C29 178.70(18) . . . . ? C24 N4 C36 P3 -1.0(3) . . . . ? C24 N4 C36 N3 -179.65(16) . . . . ? C27 N4 C24 C25 61.0(3) . . . . ? C27 N4 C24 C26 -67.3(2) . . . . ? C27 N4 C36 P3 178.41(15) . . . . ? C27 N4 C36 N3 -0.2(2) . . . . ? C28 C27 C29 N3 -176.3(2) . . . . ? C28 C27 C29 C30 3.2(3) . . . . ? C29 N3 C32 C31 78.9(2) . . . . ? C29 N3 C32 C33 -50.5(3) . . . . ? C29 N3 C36 P3 -177.73(13) . . . . ? C29 N3 C36 N4 1.1(2) . . . . ? C32 N3 C29 C27 174.99(18) . . . . ? C32 N3 C29 C30 -4.5(3) . . . . ? C32 N3 C36 P3 5.6(2) . . . . ? C32 N3 C36 N4 -175.59(16) . . . . ? C36 P3 C18 C19 -175.74(13) . . . . ? C36 P3 C18 C23 -54.41(15) . . . . ? C36 N3 C29 C27 -1.5(2) . . . . ? C36 N3 C29 C30 179.03(18) . . . . ? C36 N3 C32 C31 -105.1(2) . . . . ? C36 N3 C32 C33 125.5(2) . . . . ? C36 N4 C24 C25 -119.7(2) . . . . ? C36 N4 C24 C26 112.0(2) . . . . ? C36 N4 C27 C28 176.9(2) . . . . ? C36 N4 C27 C29 -0.7(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 -0.0000 -0.9996 -0.9992 0.0705 -0.0783 0.0873 4.9949 -3.9953 0.0028 0.5811 -0.1477 -0.1405 4.9956 -0.9972 1.0011 0.3308 -0.0701 -0.3381 1.9995 4.9976 1.9973 -0.3222 0.0959 -0.4844 -0.9989 0.9989 -0.0007 -0.1342 0.0295 0.0171 -4.9956 0.9972 -1.0011 -0.3308 0.0701 0.3381 -2.9988 1.0003 4.9975 -0.1256 0.4821 0.0009 -4.9971 -1.0000 1.9990 -0.0926 0.3066 0.3520 1.9992 -1.9998 -4.9972 0.1712 -0.4520 0.1265 4.9971 1.9997 -0.9998 0.0221 -0.2284 -0.4393 -1.9981 -3.0003 -4.9974 0.0840 -0.3324 0.4705 -1.9957 4.9940 -4.0016 -0.6160 -0.2566 -0.0028 -4.9947 0.9961 -4.0002 -0.3891 -0.1657 0.4345 2.9996 4.9967 -1.0016 -0.3363 -0.1698 -0.4603 1.0013 1.9968 -4.9993 -0.2328 -0.4236 -0.0219 4.9978 3.9981 -1.0008 -0.1578 -0.2291 -0.5496 -0.0027 -4.9946 4.0013 0.5274 0.3162 0.1472 -2.0008 -2.9964 4.9997 0.2784 0.4537 0.1493 1.9960 -4.9944 3.0019 0.5966 0.1780 0.0349