#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577314.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_1577314 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 '2(C F3 O3 S), C32 H48 N6 P2' _chemical_formula_sum 'C34 H48 F6 N6 O6 P2 S2' _chemical_formula_weight 876.84 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 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 98.2437(5) _cell_angle_gamma 90 _cell_formula_units_Z 6 _cell_length_a 7.88912(4) _cell_length_b 35.09855(17) _cell_length_c 22.64824(12) _cell_measurement_reflns_used 40785 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.4550 _cell_measurement_theta_min 2.5110 _cell_volume 6206.42(6) _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 0.994 _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 -50.00 33.00 0.50 3.00 -- -38.50 38.00 90.00 166 2 \w -117.00 -3.00 0.50 3.00 -- -38.50 -19.00 -90.00 228 3 \w -53.00 -7.00 0.50 3.00 -- -38.50 125.00-180.00 92 4 \w 35.00 93.00 0.50 3.00 -- 42.50-125.00-180.00 116 5 \w 3.00 35.00 0.50 3.00 -- 42.50 -99.00-180.00 64 6 \w 24.00 96.00 0.50 3.00 -- 42.50-125.00 -30.00 144 7 \w 75.00 121.00 0.50 15.00 -- 111.00-125.00 30.00 92 8 \w 31.00 88.00 0.50 15.00 -- 111.00 -94.00-120.00 114 9 \w 89.00 177.00 0.50 15.00 -- 111.00 30.00-150.00 176 10 \w 41.00 69.00 0.50 15.00 -- 111.00-125.00 60.00 56 11 \w 95.00 121.00 0.50 15.00 -- 111.00-125.00 60.00 52 12 \w 108.00 135.00 0.50 15.00 -- 111.00 15.00 150.00 54 13 \w 90.00 141.00 0.50 15.00 -- 111.00 45.00 150.00 102 14 \w 49.00 96.00 0.50 15.00 -- 111.00 -94.00 -60.00 94 15 \w 40.00 127.00 0.50 15.00 -- 111.00 -45.00 120.00 174 16 \w 42.00 98.00 0.50 15.00 -- 111.00 -61.00 -30.00 112 17 \w 87.00 143.00 0.50 15.00 -- 111.00 30.00 30.00 112 18 \w 39.00 82.00 0.50 15.00 -- 111.00-125.00 120.00 86 19 \w 100.00 135.00 0.50 15.00 -- 111.00 -77.00 90.00 70 20 \w 54.00 81.00 0.50 15.00 -- 111.00-125.00-120.00 54 21 \w 91.00 121.00 0.50 15.00 -- 111.00-125.00-120.00 60 22 \w 114.00 153.00 0.50 15.00 -- 111.00 45.00-120.00 78 23 \w 122.00 178.00 0.50 15.00 -- 111.00 77.00-120.00 112 24 \w 94.00 121.00 0.50 15.00 -- 111.00-125.00 -60.00 54 25 \w 94.00 170.00 0.50 15.00 -- 111.00 45.00 -30.00 152 26 \w 124.00 176.00 0.50 15.00 -- 111.00 125.00-180.00 104 27 \w 46.00 94.00 0.50 15.00 -- 111.00 -77.00 90.00 96 28 \w 88.00 170.00 0.50 15.00 -- 111.00 30.00 -60.00 164 29 \w 60.00 96.00 0.50 15.00 -- 111.00 -94.00 -90.00 72 30 \w 84.00 109.00 0.50 15.00 -- 111.00 -94.00 0.00 50 31 \w 45.00 135.00 0.50 15.00 -- 111.00 -45.00-150.00 180 32 \w 84.00 109.00 0.50 15.00 -- 111.00 -94.00 60.00 50 33 \w 66.00 121.00 0.50 15.00 -- 111.00-125.00-180.00 110 ; _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 -0.1440451000 _diffrn_orient_matrix_UB_12 -0.0286751000 _diffrn_orient_matrix_UB_13 -0.0208730000 _diffrn_orient_matrix_UB_21 -0.0977148000 _diffrn_orient_matrix_UB_22 0.0133193000 _diffrn_orient_matrix_UB_23 0.0504877000 _diffrn_orient_matrix_UB_31 -0.0928147000 _diffrn_orient_matrix_UB_32 0.0304525000 _diffrn_orient_matrix_UB_33 -0.0417248000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 68320 _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 76.745 _diffrn_reflns_theta_min 2.339 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.575 _exptl_absorpt_correction_T_max 0.847 _exptl_absorpt_correction_T_min 0.692 _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 1.408 _exptl_crystal_description block _exptl_crystal_F_000 2748 _exptl_crystal_size_max 0.187 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.081 _refine_diff_density_max 0.513 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 863 _refine_ls_number_reflns 12985 _refine_ls_number_restraints 216 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0486 _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^)+(0.0632P)^2^+6.5489P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1244 _refine_ls_wR_factor_ref 0.1264 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12179 _reflns_number_total 12985 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1064 _cod_original_cell_volume 6206.43(6) _cod_database_code 1577314 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C216 H320 Cl4 F24 N36 O36 S20 P1 ' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.819 _shelx_estimated_absorpt_t_min 0.645 _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances S2A-O5A \\sim S2B-O4B with sigma of 0.02 S2A-O4A \\sim S2B-O5B with sigma of 0.02 S2A-O6A \\sim S2B-O6B with sigma of 0.02 S2A-C49B \\sim S2B-C49A with sigma of 0.02 F4B-C49B \\sim F4A-C49A with sigma of 0.02 F5B-C49B \\sim F6A-C49A with sigma of 0.02 F6B-C49B \\sim F5A-C49A with sigma of 0.02 S2A-F4B \\sim S2B-F4A with sigma of 0.04 S2A-F5B \\sim S2B-F6A with sigma of 0.04 S2A-F6B \\sim S2B-F5A with sigma of 0.04 F4B-F5B \\sim F4A-F6A with sigma of 0.04 F4B-F6B \\sim F4A-F5A with sigma of 0.04 F5B-F6B \\sim F6A-F5A with sigma of 0.04 O5A-O4A \\sim O4B-O5B with sigma of 0.04 O5A-O6A \\sim O4B-O6B with sigma of 0.04 O5A-C49B \\sim O4B-C49A with sigma of 0.04 O4A-O6A \\sim O5B-O6B with sigma of 0.04 O4A-C49B \\sim O5B-C49A with sigma of 0.04 O6A-C49B \\sim O6B-C49A with sigma of 0.04 S3B-O7B \\sim S3A-O8A with sigma of 0.02 S3B-O9B \\sim S3A-O9A with sigma of 0.02 S3B-O8B \\sim S3A-O7A with sigma of 0.02 S3B-C50A \\sim S3A-C50B with sigma of 0.02 F7A-C50A \\sim F9B-C50B with sigma of 0.02 F9A-C50A \\sim F7B-C50B with sigma of 0.02 F8A-C50A \\sim F8B-C50B with sigma of 0.02 S3B-F7A \\sim S3A-F9B with sigma of 0.04 S3B-F9A \\sim S3A-F7B with sigma of 0.04 S3B-F8A \\sim S3A-F8B with sigma of 0.04 O7B-O9B \\sim O8A-O9A with sigma of 0.04 O7B-O8B \\sim O8A-O7A with sigma of 0.04 O7B-C50A \\sim O8A-C50B with sigma of 0.04 F7A-F9A \\sim F9B-F7B with sigma of 0.04 F7A-F8A \\sim F9B-F8B with sigma of 0.04 F9A-F8A \\sim F7B-F8B with sigma of 0.04 O9B-O8B \\sim O9A-O7A with sigma of 0.04 O9B-C50A \\sim O9A-C50B with sigma of 0.04 O8B-C50A \\sim O7A-C50B with sigma of 0.04 F7B-F8B \\sim F8B-F9B with sigma of 0.1 N7-C41A \\sim N7-C41B with sigma of 0.02 C41A-C42A \\sim C41B-C42B with sigma of 0.02 C41A-C029 \\sim C41B-C029 with sigma of 0.02 N7-C42A \\sim N7-C42B with sigma of 0.04 C42A-C029 \\sim C42B-C029 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints F7A \\sim F7B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A F8A \\sim F8B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A F9A \\sim F9B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A F7A \\sim F7B \\sim F8A \\sim F8B \\sim F9A \\sim F9B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C50A \\sim C50B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A F4B \\sim F5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A O7B \\sim O8A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A O7A \\sim O7B \\sim O8A \\sim O8B \\sim O9A \\sim O9B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(O6B) = Uanis(O4A) Uanis(C42B) = Uanis(C42A) Uanis(C41B) = Uanis(C41A) Uanis(O8A) = Uanis(O7B) = Uanis(O9A) = Uanis(O9B) = Uanis(O7A) = Uanis(O8B) Uanis(F5A) = Uanis(F4B) Uanis(O5B) = Uanis(O4A) = Uanis(O6B) = Uanis(O5A) = Uanis(O4B) = Uanis(O6A) 4. Rigid body (RIGU) restrains S3A, F7B, F8B, F9B, O7A, O8A, O9A, C50B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 S3B, F7A, F8A, F9A, O7B, O8B, O9B, C50A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(S2B)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C49A)=1- FVAR(1) Sof(S2A)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C49B)= FVAR(1) Sof(S3A)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(C50B)=1- FVAR(2) Sof(S3B)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(C50A)= FVAR(2) Sof(H02D)=Sof(H02E)=Sof(H02F)=Sof(C41B)=Sof(H41B)=Sof(C42B)=Sof(H42D)= Sof(H42E)=Sof(H42F)=1-FVAR(3) Sof(H02A)=Sof(H02B)=Sof(H02C)=Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)= Sof(H42B)=Sof(H42C)=FVAR(3) 6.a Ternary CH refined with riding coordinates: C2(H2), C9(H9), C18(H18), C25(H25), C34(H34), C41A(H41A), C41B(H41B) 6.b Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C29(H29), C30(H30), C31(H31), C32(H32), C44(H44), C45(H45), C46(H46), C47(H47) 6.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), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B, H27C), C029(H02A,H02B,H02C), C029(H02D,H02E,H02F), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42A(H42A,H42B, H42C), C42B(H42D,H42E,H42F) ; _shelx_res_file ; TITL jjw1064_a.res in P2(1)/n jjw1064.res created by SHELXL-2018/3 at 20:26:14 on 11-Jan-2026 REM Old TITL jjw1064 in P21/n #14 REM SHELXT solution in P2(1)/n REM R1 0.169, Rweak 0.006, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C51 F9 N9 O9 S6 CELL 1.54184 7.889125 35.098551 22.648239 90 98.2437 90 ZERR 6 0.000044 0.000169 0.000117 0 0.0005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O P S UNIT 204 288 36 36 36 12 12 SADI S2A O5A S2B O4B SADI S2A O4A S2B O5B SADI S2A O6A S2B O6B SADI S2A C49B S2B C49A SADI F4B C49B F4A C49A SADI F5B C49B F6A C49A SADI F6B C49B F5A C49A SADI 0.04 S2A F4B S2B F4A SADI 0.04 S2A F5B S2B F6A SADI 0.04 S2A F6B S2B F5A SADI 0.04 F4B F5B F4A F6A SADI 0.04 F4B F6B F4A F5A SADI 0.04 F5B F6B F6A F5A SADI 0.04 O5A O4A O4B O5B SADI 0.04 O5A O6A O4B O6B SADI 0.04 O5A C49B O4B C49A SADI 0.04 O4A O6A O5B O6B SADI 0.04 O4A C49B O5B C49A SADI 0.04 O6A C49B O6B C49A SADI S3B O7B S3A O8A SADI S3B O9B S3A O9A SADI S3B O8B S3A O7A SADI S3B C50A S3A C50B SADI F7A C50A F9B C50B SADI F9A C50A F7B C50B SADI F8A C50A F8B C50B SADI 0.04 S3B F7A S3A F9B SADI 0.04 S3B F9A S3A F7B SADI 0.04 S3B F8A S3A F8B SADI 0.04 O7B O9B O8A O9A SADI 0.04 O7B O8B O8A O7A SADI 0.04 O7B C50A O8A C50B SADI 0.04 F7A F9A F9B F7B SADI 0.04 F7A F8A F9B F8B SADI 0.04 F9A F8A F7B F8B SADI 0.04 O9B O8B O9A O7A SADI 0.04 O9B C50A O9A C50B SADI 0.04 O8B C50A O7A C50B SADI 0.1 F7B F8B F8B F9B SADI N7 C41A N7 C41B SADI C41A C42A C41B C42B SADI C41A C029 C41B C029 SADI 0.04 N7 C42A N7 C42B SADI 0.04 C42A C029 C42B C029 SIMU 0.01 0.02 2 F7A F7B SIMU 0.01 0.02 2 F8A F8B SIMU 0.01 0.02 2 F9A F9B SIMU 0.01 0.02 2 F7A > F9B SIMU 0.01 0.02 2 C50A C50B SIMU 0.01 0.02 2 F4B F5A SIMU 0.01 0.02 2 O7B O8A SIMU 0.01 0.02 2 O7A > O9B RIGU S3A F7B F8B F9B O7A O8A O9A C50B RIGU S3B F7A F8A F9A O7B O8B O9B C50A EADP O6B O4A EADP C42B C42A EADP C41B C41A EADP O8A O7B O9A O9B O7A O8B EADP F5A F4B EADP O5B O4A O6B O5A O4B O6A L.S. 10 0 0 PLAN 9 SIZE 0.081 0.14 0.187 TEMP 100 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.063200 6.548900 FVAR 0.16517 0.78974 0.79981 0.90779 S1 7 -0.024816 -0.029345 0.674376 11.00000 0.04509 0.01930 = 0.03295 -0.00389 0.00358 0.00113 F1 3 -0.181589 0.024212 0.607014 11.00000 0.09620 0.11422 = 0.05926 0.04500 0.02116 0.04869 F2 3 -0.312752 0.007976 0.678263 11.00000 0.03944 0.04854 = 0.09188 -0.01088 0.02625 -0.00650 F3 3 -0.089121 0.042284 0.694229 11.00000 0.04621 0.02101 = 0.13997 -0.01400 -0.00195 0.00231 O1 5 -0.012158 -0.034891 0.736601 11.00000 0.17481 0.06300 = 0.03222 0.00501 0.00575 0.06538 O2 5 0.129007 -0.017772 0.652282 11.00000 0.03693 0.03413 = 0.11339 -0.00818 0.01778 0.00076 O3 5 -0.119814 -0.057409 0.638239 11.00000 0.05962 0.04397 = 0.07443 -0.03605 0.02840 -0.02098 C48 1 -0.158912 0.013037 0.662783 11.00000 0.03150 0.03144 = 0.04344 0.00793 0.00464 -0.00260 PART 1 S2A 7 0.663479 0.311196 0.644852 21.00000 0.02641 0.02040 = 0.03612 -0.00684 0.00580 -0.00193 PART 2 S2B 7 0.719389 0.303262 0.682015 -21.00000 0.05721 0.01848 = 0.01613 -0.00190 0.01049 -0.00545 F4A 3 0.717557 0.357315 0.603402 -21.00000 0.13303 0.14972 = 0.09243 0.10253 0.07372 0.09323 PART 1 F4B 3 0.973467 0.338241 0.639214 21.00000 0.03654 0.06619 = 0.06198 -0.00874 0.01848 -0.01359 PART 2 F5A 3 0.962758 0.337105 0.634467 -21.00000 0.03654 0.06619 = 0.06198 -0.00874 0.01848 -0.01359 PART 1 F5B 3 0.812456 0.374516 0.684459 21.00000 0.06844 0.02453 = 0.11149 -0.02253 0.00343 -0.01100 PART 2 F6A 3 0.831030 0.372515 0.691993 -21.00000 0.01954 0.03931 = 0.14030 -0.03523 0.04230 -0.01107 PART 1 F6B 3 0.929029 0.323550 0.726423 21.00000 0.03972 0.07860 = 0.03734 -0.00477 -0.00474 -0.00188 O4A 5 0.544421 0.320939 0.685167 21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 PART 2 O4B 5 0.696858 0.275328 0.634073 -21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 PART 1 O5A 5 0.730869 0.272814 0.644486 21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 PART 2 O5B 5 0.831662 0.294897 0.734436 -21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 PART 1 O6A 5 0.615302 0.327279 0.586438 21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 PART 2 O6B 5 0.567730 0.312393 0.697144 -21.00000 0.04001 0.03083 = 0.04177 -0.00527 0.00211 0.00371 C49A 1 0.806736 0.344726 0.651409 -21.00000 0.04184 0.06158 = 0.08867 -0.02081 0.02171 0.00237 PART 1 C49B 1 0.854423 0.338517 0.674207 21.00000 0.02784 0.03246 = 0.04208 -0.01034 0.00967 -0.00723 PART 2 S3A 7 0.803367 0.645086 0.640572 -31.00000 0.02617 0.01635 = 0.05521 -0.00722 0.00920 0.00065 PART 1 S3B 7 0.865219 0.639566 0.679913 31.00000 0.03661 0.02270 = 0.03029 -0.00712 0.01235 -0.00206 F7A 3 0.971889 0.707052 0.715950 31.00000 0.10045 0.02625 = 0.03561 -0.00627 0.00124 -0.01566 PART 2 F7B 3 0.956194 0.708389 0.676234 -31.00000 0.11113 0.04941 = 0.14237 -0.02312 0.01057 -0.02126 PART 1 F8A 3 1.130903 0.679987 0.658076 31.00000 0.03554 0.07247 = 0.08155 0.00767 0.01165 -0.01685 PART 2 F8B 3 1.092829 0.673839 0.620239 -31.00000 0.06018 0.09485 = 0.12849 0.01370 0.02566 -0.02461 PART 1 F9A 3 0.890593 0.703962 0.622181 31.00000 0.06863 0.04809 = 0.03670 0.01671 0.00521 -0.00024 PART 2 F9B 3 1.086267 0.660444 0.714304 -31.00000 0.05099 0.10860 = 0.09079 -0.03876 -0.00958 -0.00425 O7A 5 0.871195 0.607519 0.639217 -31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 PART 1 O7B 5 0.693331 0.653186 0.684779 31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 PART 2 O8A 5 0.708899 0.645387 0.694534 -31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 PART 1 O8B 5 0.966299 0.625264 0.733471 31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 PART 2 O9A 5 0.737532 0.660151 0.582265 -31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 PART 1 O9B 5 0.883273 0.618291 0.626747 31.00000 0.05195 0.03615 = 0.03891 -0.00561 0.01097 0.00382 C50A 1 0.969307 0.684565 0.668791 31.00000 0.04178 0.02902 = 0.03609 -0.00185 0.00479 -0.00593 PART 2 C50B 1 0.991359 0.672811 0.664481 -31.00000 0.05621 0.04702 = 0.08425 -0.01524 0.00646 -0.00543 PART 0 P1 6 0.898716 0.511043 0.525921 11.00000 0.02077 0.01803 = 0.01667 0.00171 0.00202 -0.00164 N1 4 1.016964 0.527922 0.644451 11.00000 0.02569 0.02095 = 0.01889 0.00017 0.00422 0.00241 N2 4 1.162252 0.560590 0.587121 11.00000 0.01939 0.01943 = 0.02334 -0.00063 0.00120 -0.00087 N3 4 0.743477 0.534989 0.421683 11.00000 0.02968 0.02465 = 0.01946 0.00111 0.00226 0.00349 C1 1 1.030918 0.535817 0.586748 11.00000 0.02142 0.01699 = 0.01952 0.00067 0.00302 0.00112 C2 1 0.883664 0.504623 0.668401 11.00000 0.03582 0.02734 = 0.02352 0.00271 0.01099 -0.00153 AFIX 13 H2 2 0.907544 0.507583 0.711825 11.00000 -1.20000 AFIX 0 C3 1 0.707868 0.520777 0.650941 11.00000 0.03332 0.03988 = 0.04946 0.01003 0.01434 0.00015 AFIX 137 H3A 2 0.710619 0.547799 0.657572 11.00000 -1.50000 H3B 2 0.630183 0.509187 0.674573 11.00000 -1.50000 H3C 2 0.670143 0.515698 0.609489 11.00000 -1.50000 AFIX 0 C4 1 0.899049 0.462375 0.657311 11.00000 0.05436 0.02690 = 0.04464 0.01534 0.01552 0.00281 AFIX 137 H4A 2 0.865487 0.457146 0.615670 11.00000 -1.50000 H4B 2 0.825853 0.448652 0.680258 11.00000 -1.50000 H4C 2 1.015575 0.454499 0.668963 11.00000 -1.50000 AFIX 0 C5 1 1.141599 0.547459 0.680947 11.00000 0.02760 0.02705 = 0.02163 -0.00457 -0.00038 0.00610 C6 1 1.161346 0.546205 0.747467 11.00000 0.03682 0.04861 = 0.02034 -0.00718 -0.00098 0.00484 AFIX 137 H6A 2 1.059572 0.556004 0.760690 11.00000 -1.50000 H6B 2 1.257867 0.561452 0.763743 11.00000 -1.50000 H6C 2 1.179299 0.520353 0.760745 11.00000 -1.50000 AFIX 0 C7 1 1.232893 0.568025 0.645488 11.00000 0.02233 0.02451 = 0.02735 -0.00629 -0.00168 0.00359 C8 1 1.375850 0.595189 0.664784 11.00000 0.02758 0.03552 = 0.04325 -0.01299 -0.00320 -0.00232 AFIX 137 H8A 2 1.456414 0.594453 0.636807 11.00000 -1.50000 H8B 2 1.432304 0.588061 0.703603 11.00000 -1.50000 H8C 2 1.330723 0.620512 0.666346 11.00000 -1.50000 AFIX 0 C9 1 1.220652 0.576045 0.532433 11.00000 0.02659 0.02610 = 0.02794 0.00490 0.00357 -0.00644 AFIX 13 H9 2 1.139303 0.567096 0.498478 11.00000 -1.20000 AFIX 0 C10 1 1.215347 0.619571 0.531006 11.00000 0.04198 0.02563 = 0.05024 0.00909 0.00260 -0.01120 AFIX 137 H10A 2 1.106971 0.628204 0.540487 11.00000 -1.50000 H10B 2 1.229894 0.628337 0.491896 11.00000 -1.50000 H10C 2 1.305845 0.629507 0.559739 11.00000 -1.50000 AFIX 0 C11 1 1.395369 0.559776 0.524705 11.00000 0.02407 0.04601 = 0.03336 -0.00098 0.00671 -0.00763 AFIX 137 H11A 2 1.482291 0.571652 0.552713 11.00000 -1.50000 H11B 2 1.417861 0.564639 0.484844 11.00000 -1.50000 H11C 2 1.395936 0.532797 0.531695 11.00000 -1.50000 AFIX 0 C12 1 0.808474 0.549129 0.475359 11.00000 0.01884 0.02286 = 0.01842 0.00337 0.00378 -0.00011 C13 1 0.789363 0.586800 0.492135 11.00000 0.02364 0.02267 = 0.02367 0.00139 0.00386 -0.00150 AFIX 43 H13 2 0.835575 0.595385 0.529873 11.00000 -1.20000 AFIX 0 C14 1 0.698957 0.611241 0.450701 11.00000 0.02920 0.02127 = 0.03029 0.00479 0.00880 0.00111 AFIX 43 H14 2 0.683684 0.636657 0.460288 11.00000 -1.20000 AFIX 0 C15 1 0.631990 0.597355 0.395083 11.00000 0.02998 0.02956 = 0.02436 0.00974 0.00591 0.00794 AFIX 43 H15 2 0.571035 0.613223 0.366742 11.00000 -1.20000 AFIX 0 C16 1 0.657550 0.559252 0.382384 11.00000 0.03321 0.03149 = 0.01841 0.00256 0.00142 0.00634 AFIX 43 H16 2 0.612983 0.550086 0.344827 11.00000 -1.20000 AFIX 0 P2 6 -0.222360 0.177451 0.520780 11.00000 0.01975 0.01499 = 0.01648 -0.00119 0.00326 -0.00183 P3 6 -0.019163 0.156983 0.468057 11.00000 0.02098 0.01530 = 0.01820 -0.00109 0.00446 -0.00177 N4 4 0.041560 0.225846 0.584514 11.00000 0.01846 0.01587 = 0.01780 -0.00011 0.00273 -0.00145 N5 4 -0.106757 0.192286 0.640106 11.00000 0.02284 0.01618 = 0.01777 0.00016 0.00384 -0.00090 N6 4 -0.370139 0.206055 0.417935 11.00000 0.03251 0.02509 = 0.01908 0.00022 0.00203 0.00234 N7 4 -0.123541 0.139368 0.349003 11.00000 0.02751 0.01684 = 0.01922 0.00022 0.00717 -0.00072 N8 4 -0.278866 0.107397 0.404091 11.00000 0.02120 0.01605 = 0.01748 -0.00012 0.00351 -0.00050 N9 4 0.140650 0.130036 0.570445 11.00000 0.02732 0.02468 = 0.02260 0.00191 0.00383 0.00145 C17 1 -0.090167 0.200810 0.582951 11.00000 0.01996 0.01460 = 0.01756 -0.00035 0.00443 -0.00014 C18 1 -0.238403 0.167729 0.662688 11.00000 0.03147 0.01980 = 0.02477 0.00134 0.01190 -0.00405 AFIX 13 H18 2 -0.220709 0.171283 0.706055 11.00000 -1.20000 AFIX 0 C19 1 -0.208234 0.125843 0.653239 11.00000 0.04384 0.02087 = 0.04597 0.01049 0.01547 0.00079 AFIX 137 H19A 2 -0.233562 0.119987 0.611500 11.00000 -1.50000 H19B 2 -0.281259 0.111119 0.674935 11.00000 -1.50000 H19C 2 -0.090695 0.119782 0.667271 11.00000 -1.50000 AFIX 0 C20 1 -0.417501 0.181324 0.642101 11.00000 0.03072 0.03036 = 0.03513 0.00167 0.00912 -0.00270 AFIX 137 H20A 2 -0.421951 0.208534 0.645901 11.00000 -1.50000 H20B 2 -0.494377 0.169822 0.666130 11.00000 -1.50000 H20C 2 -0.450734 0.174311 0.601106 11.00000 -1.50000 AFIX 0 C21 1 0.015967 0.211681 0.677625 11.00000 0.02449 0.02226 = 0.01836 -0.00145 0.00086 0.00105 C22 1 0.028811 0.210982 0.744013 11.00000 0.03754 0.03980 = 0.01840 -0.00203 0.00153 -0.00522 AFIX 137 H22A 2 -0.069923 0.223175 0.755848 11.00000 -1.50000 H22B 2 0.130357 0.224265 0.761229 11.00000 -1.50000 H22C 2 0.034260 0.185056 0.757660 11.00000 -1.50000 AFIX 0 C23 1 0.109893 0.232630 0.643133 11.00000 0.02132 0.01964 = 0.02075 -0.00235 0.00030 0.00131 C24 1 0.253894 0.259073 0.663835 11.00000 0.02504 0.02764 = 0.02772 -0.00563 -0.00061 -0.00374 AFIX 137 H24A 2 0.336342 0.258172 0.636538 11.00000 -1.50000 H24B 2 0.307520 0.251531 0.702822 11.00000 -1.50000 H24C 2 0.210623 0.284556 0.665486 11.00000 -1.50000 AFIX 0 C25 1 0.102373 0.242155 0.530502 11.00000 0.02573 0.02237 = 0.01989 0.00134 0.00624 -0.00596 AFIX 13 H25 2 0.021596 0.233767 0.496006 11.00000 -1.20000 AFIX 0 C26 1 0.097968 0.285617 0.530667 11.00000 0.04466 0.02161 = 0.03027 0.00368 0.00329 -0.01185 AFIX 137 H26A 2 -0.010408 0.294138 0.540304 11.00000 -1.50000 H26B 2 0.113161 0.294958 0.491933 11.00000 -1.50000 H26C 2 0.188379 0.295099 0.559867 11.00000 -1.50000 AFIX 0 C27 1 0.276513 0.226097 0.522558 11.00000 0.02475 0.03907 = 0.03132 -0.00446 0.00898 -0.00685 AFIX 137 H27A 2 0.363107 0.237457 0.551289 11.00000 -1.50000 H27B 2 0.300006 0.231688 0.483037 11.00000 -1.50000 H27C 2 0.276460 0.199001 0.528327 11.00000 -1.50000 AFIX 0 C28 1 -0.308843 0.217462 0.473528 11.00000 0.01856 0.01982 = 0.01888 0.00134 0.00439 -0.00068 C29 1 -0.328585 0.254150 0.494832 11.00000 0.02174 0.02057 = 0.02356 0.00057 0.00496 -0.00132 AFIX 43 H29 2 -0.286141 0.260680 0.533960 11.00000 -1.20000 AFIX 0 C029 1 -0.032614 0.206197 0.333025 11.00000 0.05454 0.02238 = 0.04217 0.01159 0.01064 -0.00359 PART 1 AFIX 137 H02A 2 -0.151203 0.211282 0.319147 41.00000 -1.50000 H02B 2 0.037504 0.221111 0.310484 41.00000 -1.50000 H02C 2 -0.007111 0.212768 0.374494 41.00000 -1.50000 AFIX 137 PART 2 H02D 2 -0.142067 0.205762 0.308257 -41.00000 -1.50000 H02E 2 0.046202 0.221113 0.314068 -41.00000 -1.50000 H02F 2 -0.044652 0.217258 0.370967 -41.00000 -1.50000 AFIX 0 PART 0 C30 1 -0.413596 0.280695 0.455866 11.00000 0.02599 0.02010 = 0.03168 0.00319 0.00832 0.00147 AFIX 43 H30 2 -0.428812 0.305513 0.468498 11.00000 -1.20000 AFIX 0 C31 1 -0.475554 0.269844 0.397962 11.00000 0.03049 0.02960 = 0.02697 0.00951 0.00584 0.00559 AFIX 43 H31 2 -0.532002 0.287196 0.370968 11.00000 -1.20000 AFIX 0 C32 1 -0.451172 0.232368 0.381267 11.00000 0.03692 0.03314 = 0.01962 0.00279 0.00052 0.00425 AFIX 43 H32 2 -0.493459 0.225117 0.342448 11.00000 -1.20000 AFIX 0 C33 1 -0.147784 0.132555 0.405999 11.00000 0.02398 0.01428 = 0.01864 -0.00060 0.00589 -0.00066 C34 1 -0.346384 0.092499 0.457640 11.00000 0.02568 0.02103 = 0.01855 0.00042 0.00609 -0.00482 AFIX 13 H34 2 -0.267365 0.100977 0.492533 11.00000 -1.20000 AFIX 0 C35 1 -0.520648 0.109739 0.463198 11.00000 0.02542 0.03343 = 0.02926 -0.00607 0.00864 -0.00632 AFIX 137 H35A 2 -0.517193 0.136735 0.456663 11.00000 -1.50000 H35B 2 -0.548303 0.104878 0.502425 11.00000 -1.50000 H35C 2 -0.606243 0.098467 0.434006 11.00000 -1.50000 AFIX 0 C36 1 -0.347894 0.049039 0.459300 11.00000 0.04203 0.02093 = 0.02964 0.00332 0.00393 -0.00846 AFIX 137 H36A 2 -0.444169 0.039717 0.432436 11.00000 -1.50000 H36B 2 -0.356554 0.040602 0.499077 11.00000 -1.50000 H36C 2 -0.243908 0.039456 0.447432 11.00000 -1.50000 AFIX 0 C37 1 -0.338766 0.098820 0.345280 11.00000 0.02451 0.02120 = 0.01949 -0.00163 0.00087 0.00080 C38 1 -0.479540 0.071347 0.324550 11.00000 0.02679 0.03250 = 0.02661 -0.00600 -0.00104 -0.00321 AFIX 137 H38A 2 -0.434822 0.045869 0.326819 11.00000 -1.50000 H38B 2 -0.526461 0.077038 0.284032 11.00000 -1.50000 H38C 2 -0.567754 0.073491 0.349485 11.00000 -1.50000 AFIX 0 C39 1 -0.240239 0.118533 0.311059 11.00000 0.03095 0.02096 = 0.01789 -0.00021 0.00197 0.00261 C40 1 -0.239543 0.116676 0.245299 11.00000 0.04351 0.03363 = 0.01839 -0.00069 0.00366 -0.00045 AFIX 137 H40A 2 -0.244786 0.142013 0.229170 11.00000 -1.50000 H40B 2 -0.336982 0.102369 0.227137 11.00000 -1.50000 H40C 2 -0.136413 0.104452 0.237265 11.00000 -1.50000 AFIX 0 PART 1 C41A 1 0.003513 0.164403 0.325078 41.00000 0.03552 0.02133 = 0.01910 0.00069 0.01070 -0.00581 AFIX 13 H41A 2 -0.010809 0.159885 0.281949 41.00000 -1.20000 AFIX 0 PART 2 C41B 1 0.038054 0.163898 0.342599 -41.00000 0.03552 0.02133 = 0.01910 0.00069 0.01070 -0.00581 AFIX 13 H41B 2 0.098056 0.164644 0.383585 -41.00000 -1.20000 AFIX 0 PART 1 C42A 1 0.185978 0.153119 0.348816 41.00000 0.02921 0.03007 = 0.03114 -0.00110 0.01104 -0.00572 AFIX 137 H42A 2 0.212495 0.160838 0.389764 41.00000 -1.50000 H42B 2 0.263103 0.165387 0.325680 41.00000 -1.50000 H42C 2 0.197934 0.125985 0.346042 41.00000 -1.50000 AFIX 0 PART 2 C42B 1 0.162942 0.142549 0.309923 -41.00000 0.02921 0.03007 = 0.03114 -0.00110 0.01104 -0.00572 AFIX 137 H42D 2 0.173888 0.116810 0.324304 -41.00000 -1.50000 H42E 2 0.272676 0.154855 0.316786 -41.00000 -1.50000 H42F 2 0.121506 0.142434 0.267946 -41.00000 -1.50000 AFIX 0 PART 0 C43 1 0.069908 0.117586 0.516373 11.00000 0.01859 0.02029 = 0.02186 0.00182 0.00596 0.00018 C44 1 0.080093 0.080049 0.497420 11.00000 0.02539 0.02113 = 0.02976 -0.00008 0.00488 0.00042 AFIX 43 H44 2 0.032483 0.072726 0.459154 11.00000 -1.20000 AFIX 0 C45 1 0.163430 0.053912 0.537367 11.00000 0.03324 0.02095 = 0.04007 0.00438 0.00574 0.00274 AFIX 43 H45 2 0.171163 0.028490 0.526487 11.00000 -1.20000 AFIX 0 C46 1 0.234993 0.066025 0.593588 11.00000 0.03343 0.02954 = 0.03298 0.01198 0.00487 0.00477 AFIX 43 H46 2 0.290982 0.048915 0.621092 11.00000 -1.20000 AFIX 0 C47 1 0.221593 0.104120 0.608083 11.00000 0.03245 0.03291 = 0.02454 0.00479 0.00290 0.00246 AFIX 43 H47 2 0.271090 0.112178 0.645755 11.00000 -1.20000 AFIX 0 HKLF 4 REM jjw1064_a.res in P2(1)/n REM wR2 = 0.1264, GooF = S = 1.017, Restrained GooF = 1.026 for all data REM R1 = 0.0486 for 12179 Fo > 4sig(Fo) and 0.0509 for all 12985 data REM 863 parameters refined using 216 restraints END WGHT 0.0625 6.5140 REM Highest difference peak 0.513, deepest hole -0.577, 1-sigma level 0.061 Q1 1 0.7719 0.2796 0.7338 11.00000 0.05 0.46 Q2 1 0.5908 0.3030 0.7064 11.00000 0.05 0.46 Q3 1 0.2757 0.1602 0.4823 11.00000 0.05 0.43 Q4 1 -0.3909 0.1957 0.6844 11.00000 0.05 0.42 Q5 1 0.6751 0.6578 0.6577 11.00000 0.05 0.42 Q6 1 -0.1138 0.0398 0.6573 11.00000 0.05 0.41 Q7 1 0.8785 0.6184 0.7281 11.00000 0.05 0.40 Q8 1 0.6477 0.3437 0.6010 11.00000 0.05 0.40 Q9 1 -0.3054 -0.0010 0.6414 11.00000 0.05 0.39 ; _shelx_res_checksum 61760 _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 1.878 _oxdiff_exptl_absorpt_empirical_full_min 0.810 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.02482(7) -0.02934(2) 0.67438(2) 0.03264(12) Uani 1 1 d . . . . . F1 F -0.1816(3) 0.02421(7) 0.60701(9) 0.0889(8) Uani 1 1 d . . . . . F2 F -0.3128(2) 0.00798(5) 0.67826(9) 0.0583(4) Uani 1 1 d . . . . . F3 F -0.0891(2) 0.04228(4) 0.69423(11) 0.0706(6) Uani 1 1 d . . . . . O1 O -0.0122(5) -0.03489(7) 0.73660(9) 0.0909(10) Uani 1 1 d . . . . . O2 O 0.1290(2) -0.01777(5) 0.65228(12) 0.0608(6) Uani 1 1 d . . . . . O3 O -0.1198(3) -0.05741(6) 0.63824(10) 0.0575(6) Uani 1 1 d . . . . . C48 C -0.1589(3) 0.01304(6) 0.66278(11) 0.0355(5) Uani 1 1 d . . . . . S2A S 0.66348(8) 0.31120(2) 0.64485(4) 0.0275(2) Uani 0.790(2) 1 d D . P A 1 S2B S 0.7194(4) 0.30326(6) 0.68202(11) 0.0301(7) Uani 0.210(2) 1 d D . P A 2 F4A F 0.7176(17) 0.3573(4) 0.6034(5) 0.119(6) Uani 0.210(2) 1 d D . P A 2 F4B F 0.9735(10) 0.3382(4) 0.6392(7) 0.0538(11) Uani 0.790(2) 1 d D U P A 1 F5A F 0.963(4) 0.3371(15) 0.634(3) 0.0538(11) Uani 0.210(2) 1 d D U P A 2 F5B F 0.8125(8) 0.37452(16) 0.6845(4) 0.0691(17) Uani 0.790(2) 1 d D . P A 1 F6A F 0.831(2) 0.3725(6) 0.6920(12) 0.063(7) Uani 0.210(2) 1 d D . P A 2 F6B F 0.9290(2) 0.32355(7) 0.72642(8) 0.0529(5) Uani 0.790(2) 1 d D . P A 1 O4A O 0.5444(3) 0.32094(7) 0.68517(11) 0.0379(3) Uani 0.790(2) 1 d D . P A 1 O4B O 0.6969(14) 0.2753(3) 0.6341(5) 0.0379(3) Uani 0.210(2) 1 d D . P A 2 O5A O 0.7309(3) 0.27281(8) 0.64449(12) 0.0379(3) Uani 0.790(2) 1 d D . P A 1 O5B O 0.8317(10) 0.2949(2) 0.7344(3) 0.0379(3) Uani 0.210(2) 1 d D . P A 2 O6A O 0.6153(3) 0.32728(6) 0.58644(10) 0.0379(3) Uani 0.790(2) 1 d D . P A 1 O6B O 0.5677(12) 0.3124(3) 0.6971(5) 0.0379(3) Uani 0.210(2) 1 d D . P A 2 C49A C 0.807(2) 0.3447(4) 0.6514(7) 0.063(6) Uani 0.210(2) 1 d D . P A 2 C49B C 0.8544(4) 0.33852(11) 0.67421(19) 0.0337(8) Uani 0.790(2) 1 d D . P A 1 S3A S 0.8034(3) 0.64509(7) 0.64057(16) 0.0322(8) Uani 0.2002(18) 1 d D . P B 2 S3B S 0.86522(9) 0.63957(2) 0.67991(3) 0.02913(19) Uani 0.7998(18) 1 d D . P B 1 F7A F 0.9719(3) 0.70705(5) 0.71595(9) 0.0549(6) Uani 0.7998(18) 1 d D U P B 1 F7B F 0.9562(19) 0.7084(4) 0.6762(8) 0.102(4) Uani 0.2002(18) 1 d D U P B 2 F8A F 1.1309(3) 0.67999(8) 0.65808(13) 0.0629(6) Uani 0.7998(18) 1 d D U P B 1 F8B F 1.0928(16) 0.6738(4) 0.6202(7) 0.093(3) Uani 0.2002(18) 1 d D U P B 2 F9A F 0.8906(3) 0.70396(6) 0.62218(8) 0.0514(5) Uani 0.7998(18) 1 d D U P B 1 F9B F 1.0863(13) 0.6604(3) 0.7143(5) 0.085(3) Uani 0.2002(18) 1 d D U P B 2 O7A O 0.8712(15) 0.6075(3) 0.6392(5) 0.0419(3) Uani 0.2002(18) 1 d D U P B 2 O7B O 0.6933(4) 0.65319(8) 0.68478(12) 0.0419(3) Uani 0.7998(18) 1 d D U P B 1 O8A O 0.7089(16) 0.6454(3) 0.6945(5) 0.0419(3) Uani 0.2002(18) 1 d D U P B 2 O8B O 0.9663(3) 0.62526(6) 0.73347(9) 0.0419(3) Uani 0.7998(18) 1 d D . P B 1 O9A O 0.7375(12) 0.6602(2) 0.5823(3) 0.0419(3) Uani 0.2002(18) 1 d D . P B 2 O9B O 0.8833(4) 0.61829(7) 0.62675(11) 0.0419(3) Uani 0.7998(18) 1 d D U P B 1 C50A C 0.9693(5) 0.68457(11) 0.66879(15) 0.0357(7) Uani 0.7998(18) 1 d D U P B 1 C50B C 0.9914(18) 0.6728(5) 0.6645(8) 0.063(4) Uani 0.2002(18) 1 d D U P B 2 P1 P 0.89872(6) 0.51104(2) 0.52592(2) 0.01855(10) Uani 1 1 d . . . . . N1 N 1.0170(2) 0.52792(4) 0.64445(7) 0.0217(3) Uani 1 1 d . . . . . N2 N 1.16225(19) 0.56059(4) 0.58712(7) 0.0209(3) Uani 1 1 d . . . . . N3 N 0.7435(2) 0.53499(5) 0.42168(7) 0.0247(3) Uani 1 1 d . . . . . C1 C 1.0309(2) 0.53582(5) 0.58675(8) 0.0193(3) Uani 1 1 d . . . . . C2 C 0.8837(3) 0.50462(6) 0.66840(9) 0.0282(4) Uani 1 1 d . . . . . H2 H 0.907544 0.507583 0.711825 0.034 Uiso 1 1 calc R U . . . C3 C 0.7079(3) 0.52078(7) 0.65094(12) 0.0401(5) Uani 1 1 d . . . . . H3A H 0.710619 0.547799 0.657572 0.060 Uiso 1 1 calc R U . . . H3B H 0.630183 0.509187 0.674573 0.060 Uiso 1 1 calc R U . . . H3C H 0.670143 0.515698 0.609489 0.060 Uiso 1 1 calc R U . . . C4 C 0.8990(4) 0.46238(6) 0.65731(11) 0.0411(5) Uani 1 1 d . . . . . H4A H 0.865487 0.457146 0.615670 0.062 Uiso 1 1 calc R U . . . H4B H 0.825853 0.448652 0.680258 0.062 Uiso 1 1 calc R U . . . H4C H 1.015575 0.454499 0.668963 0.062 Uiso 1 1 calc R U . . . C5 C 1.1416(3) 0.54746(6) 0.68095(8) 0.0258(4) Uani 1 1 d . . . . . C6 C 1.1613(3) 0.54621(7) 0.74747(9) 0.0358(5) Uani 1 1 d . . . . . H6A H 1.059572 0.556004 0.760690 0.054 Uiso 1 1 calc R U . . . H6B H 1.257867 0.561452 0.763743 0.054 Uiso 1 1 calc R U . . . H6C H 1.179299 0.520353 0.760745 0.054 Uiso 1 1 calc R U . . . C7 C 1.2329(2) 0.56803(5) 0.64549(9) 0.0252(4) Uani 1 1 d . . . . . C8 C 1.3759(3) 0.59519(7) 0.66478(11) 0.0363(5) Uani 1 1 d . . . . . H8A H 1.456414 0.594453 0.636807 0.054 Uiso 1 1 calc R U . . . H8B H 1.432304 0.588061 0.703603 0.054 Uiso 1 1 calc R U . . . H8C H 1.330723 0.620512 0.666346 0.054 Uiso 1 1 calc R U . . . C9 C 1.2207(3) 0.57605(6) 0.53243(9) 0.0269(4) Uani 1 1 d . . . . . H9 H 1.139303 0.567096 0.498478 0.032 Uiso 1 1 calc R U . . . C10 C 1.2153(3) 0.61957(6) 0.53101(12) 0.0397(5) Uani 1 1 d . . . . . H10A H 1.106971 0.628204 0.540487 0.060 Uiso 1 1 calc R U . . . H10B H 1.229894 0.628337 0.491896 0.060 Uiso 1 1 calc R U . . . H10C H 1.305845 0.629507 0.559739 0.060 Uiso 1 1 calc R U . . . C11 C 1.3954(3) 0.55978(7) 0.52471(10) 0.0342(5) Uani 1 1 d . . . . . H11A H 1.482291 0.571652 0.552713 0.051 Uiso 1 1 calc R U . . . H11B H 1.417861 0.564639 0.484844 0.051 Uiso 1 1 calc R U . . . H11C H 1.395936 0.532797 0.531695 0.051 Uiso 1 1 calc R U . . . C12 C 0.8085(2) 0.54913(5) 0.47536(8) 0.0199(3) Uani 1 1 d . . . . . C13 C 0.7894(2) 0.58680(5) 0.49213(8) 0.0233(4) Uani 1 1 d . . . . . H13 H 0.835575 0.595385 0.529873 0.028 Uiso 1 1 calc R U . . . C14 C 0.6990(3) 0.61124(6) 0.45070(9) 0.0265(4) Uani 1 1 d . . . . . H14 H 0.683684 0.636657 0.460288 0.032 Uiso 1 1 calc R U . . . C15 C 0.6320(3) 0.59736(6) 0.39508(9) 0.0278(4) Uani 1 1 d . . . . . H15 H 0.571035 0.613223 0.366742 0.033 Uiso 1 1 calc R U . . . C16 C 0.6576(3) 0.55925(6) 0.38238(8) 0.0279(4) Uani 1 1 d . . . . . H16 H 0.612983 0.550086 0.344827 0.034 Uiso 1 1 calc R U . . . P2 P -0.22236(5) 0.17745(2) 0.52078(2) 0.01701(10) Uani 1 1 d . . . . . P3 P -0.01916(6) 0.15698(2) 0.46806(2) 0.01800(10) Uani 1 1 d . . . . . N4 N 0.04156(18) 0.22585(4) 0.58451(6) 0.0174(3) Uani 1 1 d . . . . . N5 N -0.10676(19) 0.19229(4) 0.64011(6) 0.0188(3) Uani 1 1 d . . . . . N6 N -0.3701(2) 0.20605(5) 0.41793(7) 0.0257(3) Uani 1 1 d . . . . . N7 N -0.1235(2) 0.13937(4) 0.34900(7) 0.0208(3) Uani 1 1 d D . . . . N8 N -0.27887(19) 0.10740(4) 0.40409(6) 0.0182(3) Uani 1 1 d . . . . . N9 N 0.1406(2) 0.13004(5) 0.57044(7) 0.0248(3) Uani 1 1 d . . . . . C17 C -0.0902(2) 0.20081(5) 0.58295(7) 0.0172(3) Uani 1 1 d . . . . . C18 C -0.2384(3) 0.16773(5) 0.66269(9) 0.0246(4) Uani 1 1 d . . . . . H18 H -0.220709 0.171283 0.706055 0.029 Uiso 1 1 calc R U . . . C19 C -0.2082(3) 0.12584(6) 0.65324(11) 0.0360(5) Uani 1 1 d . . . . . H19A H -0.233562 0.119987 0.611500 0.054 Uiso 1 1 calc R U . . . H19B H -0.281259 0.111119 0.674935 0.054 Uiso 1 1 calc R U . . . H19C H -0.090695 0.119782 0.667271 0.054 Uiso 1 1 calc R U . . . C20 C -0.4175(3) 0.18132(6) 0.64210(10) 0.0316(4) Uani 1 1 d . . . . . H20A H -0.421951 0.208534 0.645901 0.047 Uiso 1 1 calc R U . . . H20B H -0.494377 0.169822 0.666130 0.047 Uiso 1 1 calc R U . . . H20C H -0.450734 0.174311 0.601106 0.047 Uiso 1 1 calc R U . . . C21 C 0.0160(2) 0.21168(5) 0.67763(8) 0.0219(4) Uani 1 1 d . . . . . C22 C 0.0288(3) 0.21098(7) 0.74401(9) 0.0322(4) Uani 1 1 d . . . . . H22A H -0.069923 0.223175 0.755848 0.048 Uiso 1 1 calc R U . . . H22B H 0.130357 0.224265 0.761229 0.048 Uiso 1 1 calc R U . . . H22C H 0.034260 0.185056 0.757660 0.048 Uiso 1 1 calc R U . . . C23 C 0.1099(2) 0.23263(5) 0.64313(8) 0.0208(3) Uani 1 1 d . . . . . C24 C 0.2539(3) 0.25907(6) 0.66383(9) 0.0272(4) Uani 1 1 d . . . . . H24A H 0.336342 0.258172 0.636538 0.041 Uiso 1 1 calc R U . . . H24B H 0.307520 0.251531 0.702822 0.041 Uiso 1 1 calc R U . . . H24C H 0.210623 0.284556 0.665486 0.041 Uiso 1 1 calc R U . . . C25 C 0.1024(2) 0.24216(5) 0.53050(8) 0.0224(4) Uani 1 1 d . . . . . H25 H 0.021596 0.233767 0.496006 0.027 Uiso 1 1 calc R U . . . C26 C 0.0980(3) 0.28562(6) 0.53067(9) 0.0324(5) Uani 1 1 d . . . . . H26A H -0.010408 0.294138 0.540304 0.049 Uiso 1 1 calc R U . . . H26B H 0.113161 0.294958 0.491933 0.049 Uiso 1 1 calc R U . . . H26C H 0.188379 0.295099 0.559867 0.049 Uiso 1 1 calc R U . . . C27 C 0.2765(3) 0.22610(6) 0.52256(10) 0.0312(4) Uani 1 1 d . . . . . H27A H 0.363107 0.237457 0.551289 0.047 Uiso 1 1 calc R U . . . H27B H 0.300006 0.231688 0.483037 0.047 Uiso 1 1 calc R U . . . H27C H 0.276460 0.199001 0.528327 0.047 Uiso 1 1 calc R U . . . C28 C -0.3088(2) 0.21746(5) 0.47353(8) 0.0189(3) Uani 1 1 d . . . . . C29 C -0.3286(2) 0.25415(5) 0.49483(8) 0.0218(3) Uani 1 1 d . . . . . H29 H -0.286141 0.260680 0.533960 0.026 Uiso 1 1 calc R U . . . C029 C -0.0326(3) 0.20620(6) 0.33302(11) 0.0393(5) Uani 1 1 d D . . . . H02A H -0.151203 0.211282 0.319147 0.059 Uiso 0.908(5) 1 calc R U P C 1 H02B H 0.037504 0.221111 0.310484 0.059 Uiso 0.908(5) 1 calc R U P C 1 H02C H -0.007111 0.212768 0.374494 0.059 Uiso 0.908(5) 1 calc R U P C 1 H02D H -0.142067 0.205762 0.308257 0.059 Uiso 0.092(5) 1 calc R U P C 2 H02E H 0.046202 0.221113 0.314068 0.059 Uiso 0.092(5) 1 calc R U P C 2 H02F H -0.044652 0.217258 0.370967 0.059 Uiso 0.092(5) 1 calc R U P C 2 C30 C -0.4136(2) 0.28069(5) 0.45587(9) 0.0255(4) Uani 1 1 d . . . . . H30 H -0.428812 0.305513 0.468498 0.031 Uiso 1 1 calc R U . . . C31 C -0.4756(3) 0.26984(6) 0.39796(9) 0.0289(4) Uani 1 1 d . . . . . H31 H -0.532002 0.287196 0.370968 0.035 Uiso 1 1 calc R U . . . C32 C -0.4512(3) 0.23237(6) 0.38127(9) 0.0302(4) Uani 1 1 d . . . . . H32 H -0.493459 0.225117 0.342448 0.036 Uiso 1 1 calc R U . . . C33 C -0.1478(2) 0.13255(5) 0.40600(8) 0.0187(3) Uani 1 1 d . . . . . C34 C -0.3464(2) 0.09250(5) 0.45764(8) 0.0215(4) Uani 1 1 d . . . . . H34 H -0.267365 0.100977 0.492533 0.026 Uiso 1 1 calc R U . . . C35 C -0.5206(3) 0.10974(6) 0.46320(9) 0.0289(4) Uani 1 1 d . . . . . H35A H -0.517193 0.136735 0.456663 0.043 Uiso 1 1 calc R U . . . H35B H -0.548303 0.104878 0.502425 0.043 Uiso 1 1 calc R U . . . H35C H -0.606243 0.098467 0.434006 0.043 Uiso 1 1 calc R U . . . C36 C -0.3479(3) 0.04904(6) 0.45930(9) 0.0310(4) Uani 1 1 d . . . . . H36A H -0.444169 0.039717 0.432436 0.046 Uiso 1 1 calc R U . . . H36B H -0.356554 0.040602 0.499077 0.046 Uiso 1 1 calc R U . . . H36C H -0.243908 0.039456 0.447432 0.046 Uiso 1 1 calc R U . . . C37 C -0.3388(2) 0.09882(5) 0.34528(8) 0.0220(4) Uani 1 1 d . . . . . C38 C -0.4795(3) 0.07135(6) 0.32455(9) 0.0291(4) Uani 1 1 d . . . . . H38A H -0.434822 0.045869 0.326819 0.044 Uiso 1 1 calc R U . . . H38B H -0.526461 0.077038 0.284032 0.044 Uiso 1 1 calc R U . . . H38C H -0.567754 0.073491 0.349485 0.044 Uiso 1 1 calc R U . . . C39 C -0.2402(3) 0.11853(5) 0.31106(8) 0.0234(4) Uani 1 1 d . . . . . C40 C -0.2395(3) 0.11668(6) 0.24530(9) 0.0319(4) Uani 1 1 d . . . . . H40A H -0.244786 0.142013 0.229170 0.048 Uiso 1 1 calc R U . . . H40B H -0.336982 0.102369 0.227137 0.048 Uiso 1 1 calc R U . . . H40C H -0.136413 0.104452 0.237265 0.048 Uiso 1 1 calc R U . . . C41A C 0.0035(3) 0.16440(6) 0.32508(11) 0.0247(5) Uani 0.908(5) 1 d D . P C 1 H41A H -0.010809 0.159885 0.281949 0.030 Uiso 0.908(5) 1 calc R U P C 1 C41B C 0.038(2) 0.1639(4) 0.3426(12) 0.0247(5) Uani 0.092(5) 1 d D . P C 2 H41B H 0.098056 0.164644 0.383585 0.030 Uiso 0.092(5) 1 calc R U P C 2 C42A C 0.1860(3) 0.15312(7) 0.34882(10) 0.0295(5) Uani 0.908(5) 1 d D . P C 1 H42A H 0.212495 0.160838 0.389764 0.044 Uiso 0.908(5) 1 calc R U P C 1 H42B H 0.263103 0.165387 0.325680 0.044 Uiso 0.908(5) 1 calc R U P C 1 H42C H 0.197934 0.125985 0.346042 0.044 Uiso 0.908(5) 1 calc R U P C 1 C42B C 0.163(3) 0.1425(6) 0.3099(10) 0.0295(5) Uani 0.092(5) 1 d D . P C 2 H42D H 0.173888 0.116810 0.324304 0.044 Uiso 0.092(5) 1 calc R U P C 2 H42E H 0.272676 0.154855 0.316786 0.044 Uiso 0.092(5) 1 calc R U P C 2 H42F H 0.121506 0.142434 0.267946 0.044 Uiso 0.092(5) 1 calc R U P C 2 C43 C 0.0699(2) 0.11759(5) 0.51637(8) 0.0199(3) Uani 1 1 d . . . . . C44 C 0.0801(2) 0.08005(5) 0.49742(9) 0.0253(4) Uani 1 1 d . . . . . H44 H 0.032483 0.072726 0.459154 0.030 Uiso 1 1 calc R U . . . C45 C 0.1634(3) 0.05391(6) 0.53737(10) 0.0314(4) Uani 1 1 d . . . . . H45 H 0.171163 0.028490 0.526487 0.038 Uiso 1 1 calc R U . . . C46 C 0.2350(3) 0.06602(6) 0.59359(10) 0.0320(4) Uani 1 1 d . . . . . H46 H 0.290982 0.048915 0.621092 0.038 Uiso 1 1 calc R U . . . C47 C 0.2216(3) 0.10412(6) 0.60808(9) 0.0301(4) Uani 1 1 d . . . . . H47 H 0.271090 0.112178 0.645755 0.036 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0451(3) 0.0193(2) 0.0329(3) -0.00389(18) 0.0036(2) 0.00113(19) F1 0.0962(16) 0.1142(18) 0.0593(12) 0.0450(12) 0.0212(11) 0.0487(14) F2 0.0394(8) 0.0485(9) 0.0919(13) -0.0109(8) 0.0262(8) -0.0065(7) F3 0.0462(9) 0.0210(7) 0.1400(18) -0.0140(9) -0.0020(10) 0.0023(6) O1 0.175(3) 0.0630(14) 0.0322(10) 0.0050(9) 0.0057(14) 0.0654(17) O2 0.0369(10) 0.0341(9) 0.1134(19) -0.0082(10) 0.0178(11) 0.0008(7) O3 0.0596(12) 0.0440(10) 0.0744(14) -0.0361(10) 0.0284(10) -0.0210(9) C48 0.0315(11) 0.0314(11) 0.0434(12) 0.0079(9) 0.0046(9) -0.0026(8) S2A 0.0264(3) 0.0204(3) 0.0361(5) -0.0068(3) 0.0058(3) -0.0019(2) S2B 0.0572(16) 0.0185(10) 0.0161(13) -0.0019(8) 0.0105(12) -0.0055(10) F4A 0.133(10) 0.150(12) 0.092(8) 0.103(9) 0.074(8) 0.093(10) F4B 0.0365(14) 0.0662(13) 0.062(3) -0.0087(14) 0.0185(18) -0.0136(12) F5A 0.0365(14) 0.0662(13) 0.062(3) -0.0087(14) 0.0185(18) -0.0136(12) F5B 0.068(3) 0.025(2) 0.111(3) -0.0225(19) 0.003(2) -0.0110(17) F6A 0.020(5) 0.039(9) 0.140(18) -0.035(9) 0.042(8) -0.011(4) F6B 0.0397(10) 0.0786(15) 0.0373(10) -0.0048(9) -0.0047(8) -0.0019(9) O4A 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) O4B 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) O5A 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) O5B 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) O6A 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) O6B 0.0400(7) 0.0308(6) 0.0418(8) -0.0053(5) 0.0021(5) 0.0037(5) C49A 0.042(10) 0.062(11) 0.089(17) -0.021(11) 0.022(10) 0.002(8) C49B 0.0278(19) 0.0325(16) 0.042(2) -0.0103(14) 0.0097(14) -0.0072(14) S3A 0.0262(13) 0.0164(11) 0.055(2) -0.0072(11) 0.0092(13) 0.0006(9) S3B 0.0366(4) 0.0227(3) 0.0303(4) -0.0071(2) 0.0123(3) -0.0021(2) F7A 0.1004(17) 0.0262(9) 0.0356(10) -0.0063(8) 0.0012(11) -0.0157(9) F7B 0.111(8) 0.049(5) 0.142(9) -0.023(6) 0.011(7) -0.021(5) F8A 0.0355(11) 0.0725(16) 0.0816(17) 0.0077(14) 0.0117(11) -0.0168(10) F8B 0.060(6) 0.095(7) 0.128(8) 0.014(7) 0.026(6) -0.025(5) F9A 0.0686(13) 0.0481(11) 0.0367(10) 0.0167(8) 0.0052(9) -0.0002(9) F9B 0.051(5) 0.109(7) 0.091(6) -0.039(5) -0.010(4) -0.004(5) O7A 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) O7B 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) O8A 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) O8B 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) O9A 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) O9B 0.0520(7) 0.0361(8) 0.0389(8) -0.0056(5) 0.0110(6) 0.0038(6) C50A 0.0418(16) 0.0290(18) 0.0361(15) -0.0019(13) 0.0048(12) -0.0059(14) C50B 0.056(6) 0.047(6) 0.084(7) -0.015(6) 0.006(5) -0.005(6) P1 0.0208(2) 0.0180(2) 0.0167(2) 0.00171(15) 0.00202(16) -0.00164(16) N1 0.0257(8) 0.0209(7) 0.0189(7) 0.0002(6) 0.0042(6) 0.0024(6) N2 0.0194(7) 0.0194(7) 0.0233(7) -0.0006(6) 0.0012(6) -0.0009(6) N3 0.0297(8) 0.0246(8) 0.0195(7) 0.0011(6) 0.0023(6) 0.0035(6) C1 0.0214(8) 0.0170(8) 0.0195(8) 0.0007(6) 0.0030(6) 0.0011(6) C2 0.0358(11) 0.0273(10) 0.0235(9) 0.0027(7) 0.0110(8) -0.0015(8) C3 0.0333(11) 0.0399(12) 0.0495(14) 0.0100(10) 0.0143(10) 0.0001(9) C4 0.0544(14) 0.0269(11) 0.0446(13) 0.0153(9) 0.0155(11) 0.0028(10) C5 0.0276(9) 0.0270(9) 0.0216(9) -0.0046(7) -0.0004(7) 0.0061(7) C6 0.0368(11) 0.0486(13) 0.0203(9) -0.0072(9) -0.0010(8) 0.0048(10) C7 0.0223(9) 0.0245(9) 0.0273(9) -0.0063(7) -0.0017(7) 0.0036(7) C8 0.0276(10) 0.0355(11) 0.0432(12) -0.0130(9) -0.0032(9) -0.0023(9) C9 0.0266(10) 0.0261(9) 0.0279(10) 0.0049(7) 0.0036(8) -0.0064(7) C10 0.0420(12) 0.0256(11) 0.0502(14) 0.0091(9) 0.0026(10) -0.0112(9) C11 0.0241(10) 0.0460(13) 0.0334(11) -0.0010(9) 0.0067(8) -0.0076(9) C12 0.0188(8) 0.0229(8) 0.0184(8) 0.0034(6) 0.0038(6) -0.0001(6) C13 0.0236(9) 0.0227(9) 0.0237(9) 0.0014(7) 0.0039(7) -0.0015(7) C14 0.0292(10) 0.0213(9) 0.0303(10) 0.0048(7) 0.0088(8) 0.0011(7) C15 0.0300(10) 0.0296(10) 0.0244(9) 0.0097(7) 0.0059(8) 0.0079(8) C16 0.0332(10) 0.0315(10) 0.0184(8) 0.0026(7) 0.0014(7) 0.0063(8) P2 0.0197(2) 0.0150(2) 0.0165(2) -0.00119(15) 0.00326(15) -0.00183(15) P3 0.0210(2) 0.0153(2) 0.0182(2) -0.00109(15) 0.00446(16) -0.00177(15) N4 0.0185(7) 0.0159(6) 0.0178(7) -0.0001(5) 0.0027(5) -0.0015(5) N5 0.0228(7) 0.0162(7) 0.0178(7) 0.0002(5) 0.0038(6) -0.0009(5) N6 0.0325(9) 0.0251(8) 0.0191(7) 0.0002(6) 0.0020(6) 0.0023(6) N7 0.0275(8) 0.0168(7) 0.0192(7) 0.0002(5) 0.0072(6) -0.0007(6) N8 0.0212(7) 0.0160(7) 0.0175(7) -0.0001(5) 0.0035(6) -0.0005(5) N9 0.0273(8) 0.0247(8) 0.0226(8) 0.0019(6) 0.0038(6) 0.0015(6) C17 0.0200(8) 0.0146(7) 0.0176(8) -0.0003(6) 0.0044(6) -0.0001(6) C18 0.0315(10) 0.0198(9) 0.0248(9) 0.0013(7) 0.0119(8) -0.0040(7) C19 0.0438(12) 0.0209(10) 0.0460(13) 0.0105(9) 0.0155(10) 0.0008(8) C20 0.0307(10) 0.0304(10) 0.0351(11) 0.0017(8) 0.0091(8) -0.0027(8) C21 0.0245(9) 0.0223(8) 0.0184(8) -0.0015(7) 0.0009(7) 0.0011(7) C22 0.0375(11) 0.0398(11) 0.0184(9) -0.0020(8) 0.0015(8) -0.0052(9) C23 0.0213(8) 0.0196(8) 0.0208(8) -0.0023(6) 0.0003(7) 0.0013(7) C24 0.0250(9) 0.0276(9) 0.0277(9) -0.0056(7) -0.0006(7) -0.0037(7) C25 0.0257(9) 0.0224(9) 0.0199(8) 0.0013(7) 0.0062(7) -0.0060(7) C26 0.0447(12) 0.0216(9) 0.0303(10) 0.0037(8) 0.0033(9) -0.0118(8) C27 0.0247(10) 0.0391(11) 0.0313(10) -0.0045(8) 0.0090(8) -0.0069(8) C28 0.0186(8) 0.0198(8) 0.0189(8) 0.0013(6) 0.0044(6) -0.0007(6) C29 0.0217(8) 0.0206(8) 0.0236(8) 0.0006(7) 0.0050(7) -0.0013(7) C029 0.0545(14) 0.0224(10) 0.0422(12) 0.0116(9) 0.0106(11) -0.0036(9) C30 0.0260(9) 0.0201(9) 0.0317(10) 0.0032(7) 0.0083(8) 0.0015(7) C31 0.0305(10) 0.0296(10) 0.0270(9) 0.0095(8) 0.0058(8) 0.0056(8) C32 0.0369(11) 0.0331(10) 0.0196(9) 0.0028(8) 0.0005(8) 0.0042(8) C33 0.0240(8) 0.0143(7) 0.0186(8) -0.0006(6) 0.0059(6) -0.0007(6) C34 0.0257(9) 0.0210(8) 0.0186(8) 0.0004(6) 0.0061(7) -0.0048(7) C35 0.0254(10) 0.0334(10) 0.0293(10) -0.0061(8) 0.0086(8) -0.0063(8) C36 0.0420(12) 0.0209(9) 0.0296(10) 0.0033(7) 0.0039(9) -0.0085(8) C37 0.0245(9) 0.0212(8) 0.0195(8) -0.0016(7) 0.0009(7) 0.0008(7) C38 0.0268(10) 0.0325(10) 0.0266(9) -0.0060(8) -0.0010(8) -0.0032(8) C39 0.0310(10) 0.0210(8) 0.0179(8) -0.0002(7) 0.0020(7) 0.0026(7) C40 0.0435(12) 0.0336(11) 0.0184(9) -0.0007(8) 0.0037(8) -0.0004(9) C41A 0.0355(12) 0.0213(9) 0.0191(12) 0.0007(8) 0.0107(9) -0.0058(8) C41B 0.0355(12) 0.0213(9) 0.0191(12) 0.0007(8) 0.0107(9) -0.0058(8) C42A 0.0292(11) 0.0301(11) 0.0311(12) -0.0011(9) 0.0110(9) -0.0057(9) C42B 0.0292(11) 0.0301(11) 0.0311(12) -0.0011(9) 0.0110(9) -0.0057(9) C43 0.0186(8) 0.0203(8) 0.0219(8) 0.0018(7) 0.0060(6) 0.0002(6) C44 0.0254(9) 0.0211(9) 0.0298(10) -0.0001(7) 0.0049(7) 0.0004(7) C45 0.0332(11) 0.0209(9) 0.0401(11) 0.0044(8) 0.0057(9) 0.0027(8) C46 0.0334(11) 0.0295(10) 0.0330(10) 0.0120(8) 0.0049(8) 0.0048(8) C47 0.0324(10) 0.0329(10) 0.0245(9) 0.0048(8) 0.0029(8) 0.0025(8) 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 -3 12 10 0.0568 1 0 -5 0.0424 0 -1 0 0.0922 -2 17 9 0.0717 -1 12 12 0.0577 0 -2 5 0.0535 -1 5 -3 0.0739 -2 5 -2 0.0704 -5 1 -1 0.0729 -1 -5 3 0.0842 1 -5 1 0.0934 1 0 5 0.0497 0 5 -1 0.0821 1 0 1 0.0500 2 5 0 0.0757 -2 -5 3 0.0826 5 -1 1 0.0550 0 0 -1 0.0220 0 -5 -4 0.0594 0 -5 3 0.0805 -2 9 12 0.0558 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 O1 S1 O2 116.39(19) . . ? O1 S1 O3 115.76(17) . . ? O1 S1 C48 102.29(12) . . ? O2 S1 C48 102.77(11) . . ? O3 S1 O2 113.39(13) . . ? O3 S1 C48 103.60(12) . . ? F1 C48 S1 112.30(19) . . ? F1 C48 F2 107.0(2) . . ? F1 C48 F3 106.0(2) . . ? F2 C48 S1 112.83(16) . . ? F2 C48 F3 106.8(2) . . ? F3 C48 S1 111.56(16) . . ? O4A S2A O5A 119.81(17) . . ? O4A S2A C49B 102.88(17) . . ? O5A S2A C49B 101.88(17) . . ? O6A S2A O4A 112.28(13) . . ? O6A S2A O5A 114.11(15) . . ? O6A S2A C49B 102.94(16) . . ? O4B S2B C49A 105.7(7) . . ? O5B S2B O4B 118.9(5) . . ? O5B S2B C49A 105.4(6) . . ? O6B S2B O4B 109.7(7) . . ? O6B S2B O5B 108.3(6) . . ? O6B S2B C49A 108.3(7) . . ? F4A C49A S2B 114.3(11) . . ? F4A C49A F5A 104(3) . . ? F4A C49A F6A 109.8(18) . . ? F5A C49A S2B 111(2) . . ? F6A C49A S2B 110.6(14) . . ? F6A C49A F5A 107(2) . . ? F4B C49B S2A 113.6(6) . . ? F4B C49B F5B 109.2(7) . . ? F4B C49B F6B 105.4(7) . . ? F5B C49B S2A 110.3(4) . . ? F5B C49B F6B 107.7(5) . . ? F6B C49B S2A 110.3(3) . . ? O7A S3A O8A 104.6(6) . . ? O7A S3A O9A 113.9(6) . . ? O7A S3A C50B 102.2(7) . . ? O8A S3A C50B 103.5(8) . . ? O9A S3A O8A 125.3(6) . . ? O9A S3A C50B 104.5(7) . . ? O7B S3B C50A 99.76(17) . . ? O8B S3B O7B 117.31(14) . . ? O8B S3B C50A 102.30(15) . . ? O9B S3B O7B 115.96(18) . . ? O9B S3B O8B 114.41(14) . . ? O9B S3B C50A 103.54(16) . . ? F7A C50A S3B 111.2(2) . . ? F7A C50A F8A 108.2(3) . . ? F7A C50A F9A 106.6(3) . . ? F8A C50A S3B 112.4(3) . . ? F9A C50A S3B 112.7(2) . . ? F9A C50A F8A 105.4(3) . . ? F7B C50B S3A 112.8(12) . . ? F7B C50B F8B 106.6(14) . . ? F7B C50B F9B 104.3(15) . . ? F8B C50B S3A 109.8(11) . . ? F9B C50B S3A 114.8(11) . . ? F9B C50B F8B 108.1(13) . . ? C1 P1 P1 100.73(6) . 3_766 ? C1 P1 C12 104.62(8) . . ? C12 P1 P1 99.56(6) . 3_766 ? C1 N1 C2 128.35(16) . . ? C1 N1 C5 109.14(16) . . ? C5 N1 C2 122.35(16) . . ? C1 N2 C7 109.31(16) . . ? C1 N2 C9 123.99(15) . . ? C7 N2 C9 126.68(16) . . ? C16 N3 C12 117.12(17) . . ? N1 C1 P1 120.91(13) . . ? N2 C1 P1 131.75(14) . . ? N2 C1 N1 107.07(15) . . ? N1 C2 H2 105.2 . . ? N1 C2 C3 111.73(17) . . ? N1 C2 C4 113.52(17) . . ? C3 C2 H2 105.2 . . ? C3 C2 C4 114.9(2) . . ? C4 C2 H2 105.2 . . ? 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 123.68(19) . . ? C7 C5 N1 107.67(16) . . ? C7 C5 C6 128.60(19) . . ? 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 125.71(19) . . ? C5 C7 N2 106.80(17) . . ? C5 C7 C8 127.41(19) . . ? 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 106.9 . . ? N2 C9 C10 111.84(18) . . ? N2 C9 C11 110.65(16) . . ? C10 C9 H9 106.9 . . ? C11 C9 H9 106.9 . . ? C11 C9 C10 113.22(18) . . ? 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 . . ? N3 C12 P1 111.01(13) . . ? N3 C12 C13 123.78(17) . . ? C13 C12 P1 124.73(14) . . ? C12 C13 H13 121.1 . . ? C12 C13 C14 117.89(18) . . ? C14 C13 H13 121.1 . . ? C13 C14 H14 120.4 . . ? C15 C14 C13 119.29(18) . . ? C15 C14 H14 120.4 . . ? C14 C15 H15 120.7 . . ? C14 C15 C16 118.70(18) . . ? C16 C15 H15 120.7 . . ? N3 C16 C15 123.22(18) . . ? N3 C16 H16 118.4 . . ? C15 C16 H16 118.4 . . ? C17 P2 P3 100.45(6) . . ? C17 P2 C28 103.29(8) . . ? C28 P2 P3 99.69(6) . . ? C33 P3 P2 101.48(6) . . ? C33 P3 C43 103.17(8) . . ? C43 P3 P2 99.49(6) . . ? C17 N4 C23 109.19(14) . . ? C17 N4 C25 124.22(14) . . ? C23 N4 C25 126.57(15) . . ? C17 N5 C18 128.46(15) . . ? C17 N5 C21 109.02(15) . . ? C21 N5 C18 122.46(15) . . ? C32 N6 C28 116.78(17) . . ? C33 N7 C39 109.17(15) . . ? C33 N7 C41A 130.15(17) . . ? C33 N7 C41B 114.5(10) . . ? C39 N7 C41A 120.68(16) . . ? C39 N7 C41B 135.8(10) . . ? C33 N8 C34 124.30(15) . . ? C33 N8 C37 109.06(15) . . ? C37 N8 C34 126.63(15) . . ? C47 N9 C43 117.09(17) . . ? N4 C17 P2 131.49(13) . . ? N5 C17 P2 121.10(13) . . ? N5 C17 N4 107.27(15) . . ? N5 C18 H18 105.3 . . ? N5 C18 C19 112.43(16) . . ? N5 C18 C20 112.31(16) . . ? C19 C18 H18 105.3 . . ? C20 C18 H18 105.3 . . ? C20 C18 C19 115.22(18) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 C22 123.71(17) . . ? C23 C21 N5 107.76(15) . . ? C23 C21 C22 128.38(18) . . ? 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 . . ? N4 C23 C24 125.83(17) . . ? C21 C23 N4 106.75(15) . . ? C21 C23 C24 127.38(17) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 H25 106.8 . . ? N4 C25 C26 111.82(15) . . ? N4 C25 C27 110.95(16) . . ? C26 C25 H25 106.8 . . ? C27 C25 H25 106.8 . . ? C27 C25 C26 113.11(17) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 C28 P2 111.83(13) . . ? N6 C28 C29 123.89(17) . . ? C29 C28 P2 123.79(14) . . ? C28 C29 H29 121.0 . . ? C30 C29 C28 117.94(17) . . ? C30 C29 H29 121.0 . . ? H02A C029 H02B 109.5 . . ? H02A C029 H02C 109.5 . . ? H02B C029 H02C 109.5 . . ? H02D C029 H02E 109.5 . . ? H02D C029 H02F 109.5 . . ? H02E C029 H02F 109.5 . . ? C41A C029 H02A 109.5 . . ? C41A C029 H02B 109.5 . . ? C41A C029 H02C 109.5 . . ? C41B C029 H02D 109.5 . . ? C41B C029 H02E 109.5 . . ? C41B C029 H02F 109.5 . . ? C29 C30 H30 120.3 . . ? C31 C30 C29 119.34(18) . . ? C31 C30 H30 120.3 . . ? C30 C31 H31 120.9 . . ? C30 C31 C32 118.29(18) . . ? C32 C31 H31 120.9 . . ? N6 C32 C31 123.75(18) . . ? N6 C32 H32 118.1 . . ? C31 C32 H32 118.1 . . ? N7 C33 P3 120.84(13) . . ? N7 C33 N8 107.23(15) . . ? N8 C33 P3 131.90(13) . . ? N8 C34 H34 106.9 . . ? N8 C34 C35 111.13(15) . . ? N8 C34 C36 112.11(15) . . ? C35 C34 H34 106.9 . . ? C35 C34 C36 112.62(16) . . ? C36 C34 H34 106.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N8 C37 C38 125.42(17) . . ? C39 C37 N8 107.08(16) . . ? C39 C37 C38 127.43(17) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 123.29(18) . . ? C37 C39 N7 107.44(16) . . ? C37 C39 C40 129.04(18) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N7 C41A C029 112.38(18) . . ? N7 C41A H41A 106.2 . . ? N7 C41A C42A 111.76(18) . . ? C029 C41A H41A 106.2 . . ? C029 C41A C42A 113.4(2) . . ? C42A C41A H41A 106.2 . . ? N7 C41B C029 104.6(10) . . ? N7 C41B H41B 102.5 . . ? C029 C41B H41B 102.5 . . ? C42B C41B N7 111.7(14) . . ? C42B C41B C029 129.5(16) . . ? C42B C41B H41B 102.5 . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42B 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42E 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? N9 C43 P3 111.78(13) . . ? N9 C43 C44 123.65(17) . . ? C44 C43 P3 124.22(14) . . ? C43 C44 H44 121.0 . . ? C45 C44 C43 117.92(19) . . ? C45 C44 H44 121.0 . . ? C44 C45 H45 120.3 . . ? C46 C45 C44 119.34(19) . . ? C46 C45 H45 120.3 . . ? C45 C46 H46 120.7 . . ? C45 C46 C47 118.69(19) . . ? C47 C46 H46 120.7 . . ? N9 C47 C46 123.3(2) . . ? N9 C47 H47 118.4 . . ? C46 C47 H47 118.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O1 1.412(2) . ? S1 O2 1.436(2) . ? S1 O3 1.4233(18) . ? S1 C48 1.822(2) . ? F1 C48 1.310(3) . ? F2 C48 1.323(3) . ? F3 C48 1.324(3) . ? S2A O4A 1.442(3) . ? S2A O5A 1.449(3) . ? S2A O6A 1.438(2) . ? S2A C49B 1.829(3) . ? S2B O4B 1.455(10) . ? S2B O5B 1.407(8) . ? S2B O6B 1.330(10) . ? S2B C49A 1.792(13) . ? F4A C49A 1.286(15) . ? F4B C49B 1.313(8) . ? F5A C49A 1.367(18) . ? F5B C49B 1.335(6) . ? F6A C49A 1.335(16) . ? F6B C49B 1.350(4) . ? S3A O7A 1.425(9) . ? S3A O8A 1.520(10) . ? S3A O9A 1.448(8) . ? S3A C50B 1.791(14) . ? S3B O7B 1.457(3) . ? S3B O8B 1.443(2) . ? S3B O9B 1.441(2) . ? S3B C50A 1.814(4) . ? F7A C50A 1.326(4) . ? F7B C50B 1.315(14) . ? F8A C50A 1.341(4) . ? F8B C50B 1.370(16) . ? F9A C50A 1.332(4) . ? F9B C50B 1.334(16) . ? P1 P1 2.2520(9) 3_766 ? P1 C1 1.8247(18) . ? P1 C12 1.8361(18) . ? N1 C1 1.356(2) . ? N1 C2 1.494(2) . ? N1 C5 1.374(3) . ? N2 C1 1.352(2) . ? N2 C7 1.384(2) . ? N2 C9 1.485(2) . ? N3 C12 1.345(2) . ? N3 C16 1.343(2) . ? C2 H2 0.9800 . ? C2 C3 1.498(3) . ? C2 C4 1.512(3) . ? 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 1.493(3) . ? C5 C7 1.360(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.494(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9 0.9800 . ? C9 C10 1.528(3) . ? C9 C11 1.525(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 C13 1.390(3) . ? C13 H13 0.9300 . ? C13 C14 1.390(3) . ? C14 H14 0.9300 . ? C14 C15 1.383(3) . ? C15 H15 0.9300 . ? C15 C16 1.389(3) . ? C16 H16 0.9300 . ? P2 P3 2.2496(6) . ? P2 C17 1.8225(18) . ? P2 C28 1.8367(18) . ? P3 C33 1.8252(18) . ? P3 C43 1.8392(18) . ? N4 C17 1.358(2) . ? N4 C23 1.380(2) . ? N4 C25 1.491(2) . ? N5 C17 1.353(2) . ? N5 C18 1.495(2) . ? N5 C21 1.374(2) . ? N6 C28 1.343(2) . ? N6 C32 1.341(3) . ? N7 C33 1.353(2) . ? N7 C39 1.376(2) . ? N7 C41A 1.492(3) . ? N7 C41B 1.562(17) . ? N8 C33 1.356(2) . ? N8 C34 1.488(2) . ? N8 C37 1.381(2) . ? N9 C43 1.344(2) . ? N9 C47 1.344(3) . ? C18 H18 0.9800 . ? C18 C19 1.509(3) . ? C18 C20 1.501(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.493(3) . ? C21 C23 1.366(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.490(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.526(3) . ? C25 C27 1.519(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.392(3) . ? C29 H29 0.9300 . ? C29 C30 1.388(3) . ? C029 H02A 0.9600 . ? C029 H02B 0.9600 . ? C029 H02C 0.9600 . ? C029 H02D 0.9600 . ? C029 H02E 0.9600 . ? C029 H02F 0.9600 . ? C029 C41A 1.510(3) . ? C029 C41B 1.590(16) . ? C30 H30 0.9300 . ? C30 C31 1.386(3) . ? C31 H31 0.9300 . ? C31 C32 1.390(3) . ? C32 H32 0.9300 . ? C34 H34 0.9800 . ? C34 C35 1.524(3) . ? C34 C36 1.526(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.495(3) . ? C37 C39 1.362(3) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.492(3) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41A H41A 0.9800 . ? C41A C42A 1.515(3) . ? C41B H41B 0.9800 . ? C41B C42B 1.513(17) . ? C42A H42A 0.9600 . ? C42A H42B 0.9600 . ? C42A H42C 0.9600 . ? C42B H42D 0.9600 . ? C42B H42E 0.9600 . ? C42B H42F 0.9600 . ? C43 C44 1.392(3) . ? C44 H44 0.9300 . ? C44 C45 1.386(3) . ? C45 H45 0.9300 . ? C45 C46 1.384(3) . ? C46 H46 0.9300 . ? C46 C47 1.384(3) . ? C47 H47 0.9300 . ? 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 O1 S1 C48 F1 177.5(2) . . . . ? O1 S1 C48 F2 -61.5(2) . . . . ? O1 S1 C48 F3 58.6(2) . . . . ? O2 S1 C48 F1 56.4(2) . . . . ? O2 S1 C48 F2 177.43(19) . . . . ? O2 S1 C48 F3 -62.4(2) . . . . ? O3 S1 C48 F1 -61.8(2) . . . . ? O3 S1 C48 F2 59.2(2) . . . . ? O3 S1 C48 F3 179.33(19) . . . . ? O4A S2A C49B F4B -170.9(7) . . . . ? O4A S2A C49B F5B -47.9(5) . . . . ? O4A S2A C49B F6B 71.0(3) . . . . ? O4B S2B C49A F4A 54.9(14) . . . . ? O4B S2B C49A F5A -62(3) . . . . ? O4B S2B C49A F6A 179.4(14) . . . . ? O5A S2A C49B F4B 64.4(8) . . . . ? O5A S2A C49B F5B -172.6(5) . . . . ? O5A S2A C49B F6B -53.7(3) . . . . ? O5B S2B C49A F4A -178.3(11) . . . . ? O5B S2B C49A F5A 65(3) . . . . ? O5B S2B C49A F6A -53.8(15) . . . . ? O6A S2A C49B F4B -54.1(7) . . . . ? O6A S2A C49B F5B 68.9(5) . . . . ? O6A S2A C49B F6B -172.2(2) . . . . ? O6B S2B C49A F4A -62.6(14) . . . . ? O6B S2B C49A F5A -180(3) . . . . ? O6B S2B C49A F6A 61.9(16) . . . . ? O7A S3A C50B F7B -171.9(14) . . . . ? O7A S3A C50B F8B 69.4(12) . . . . ? O7A S3A C50B F9B -52.6(13) . . . . ? O7B S3B C50A F7A 63.5(3) . . . . ? O7B S3B C50A F8A -175.1(3) . . . . ? O7B S3B C50A F9A -56.2(3) . . . . ? O8A S3A C50B F7B -63.4(15) . . . . ? O8A S3A C50B F8B 177.9(11) . . . . ? O8A S3A C50B F9B 55.9(13) . . . . ? O8B S3B C50A F7A -57.5(3) . . . . ? O8B S3B C50A F8A 64.0(3) . . . . ? O8B S3B C50A F9A -177.1(2) . . . . ? O9A S3A C50B F7B 69.1(15) . . . . ? O9A S3A C50B F8B -49.6(12) . . . . ? O9A S3A C50B F9B -171.6(11) . . . . ? O9B S3B C50A F7A -176.6(3) . . . . ? O9B S3B C50A F8A -55.2(3) . . . . ? O9B S3B C50A F9A 63.7(3) . . . . ? P1 P1 C1 N1 -126.25(14) 3_766 . . . ? P1 P1 C1 N2 47.00(18) 3_766 . . . ? P1 P1 C12 N3 60.68(13) 3_766 . . . ? P1 P1 C12 C13 -127.04(15) 3_766 . . . ? P1 C12 C13 C14 -171.88(14) . . . . ? N1 C5 C7 N2 -0.2(2) . . . . ? N1 C5 C7 C8 176.76(19) . . . . ? N3 C12 C13 C14 -0.6(3) . . . . ? C1 P1 C12 N3 164.50(13) . . . . ? C1 P1 C12 C13 -23.22(18) . . . . ? C1 N1 C2 C3 -60.3(3) . . . . ? C1 N1 C2 C4 71.6(3) . . . . ? C1 N1 C5 C6 178.42(18) . . . . ? C1 N1 C5 C7 0.6(2) . . . . ? C1 N2 C7 C5 -0.3(2) . . . . ? C1 N2 C7 C8 -177.32(18) . . . . ? C1 N2 C9 C10 122.7(2) . . . . ? C1 N2 C9 C11 -110.0(2) . . . . ? C2 N1 C1 P1 -10.6(3) . . . . ? C2 N1 C1 N2 174.65(17) . . . . ? C2 N1 C5 C6 2.6(3) . . . . ? C2 N1 C5 C7 -175.17(17) . . . . ? C5 N1 C1 P1 173.93(13) . . . . ? C5 N1 C1 N2 -0.8(2) . . . . ? C5 N1 C2 C3 114.7(2) . . . . ? C5 N1 C2 C4 -113.5(2) . . . . ? C6 C5 C7 N2 -177.84(19) . . . . ? C6 C5 C7 C8 -0.9(3) . . . . ? C7 N2 C1 P1 -173.25(14) . . . . ? C7 N2 C1 N1 0.7(2) . . . . ? C7 N2 C9 C10 -58.9(2) . . . . ? C7 N2 C9 C11 68.3(2) . . . . ? C9 N2 C1 P1 5.4(3) . . . . ? C9 N2 C1 N1 179.30(16) . . . . ? C9 N2 C7 C5 -178.88(17) . . . . ? C9 N2 C7 C8 4.1(3) . . . . ? C12 P1 C1 N1 130.80(15) . . . . ? C12 P1 C1 N2 -55.95(19) . . . . ? C12 N3 C16 C15 -0.9(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 N3 0.5(3) . . . . ? C16 N3 C12 P1 173.29(15) . . . . ? C16 N3 C12 C13 0.9(3) . . . . ? P2 P3 C33 N7 131.44(14) . . . . ? P2 P3 C33 N8 -46.05(18) . . . . ? P2 P3 C43 N9 -63.11(13) . . . . ? P2 P3 C43 C44 123.53(15) . . . . ? P2 C28 C29 C30 -172.70(14) . . . . ? P3 P2 C17 N4 47.18(17) . . . . ? P3 P2 C17 N5 -127.92(13) . . . . ? P3 P2 C28 N6 59.30(13) . . . . ? P3 P2 C28 C29 -128.46(15) . . . . ? P3 C43 C44 C45 174.66(15) . . . . ? N5 C21 C23 N4 0.4(2) . . . . ? N5 C21 C23 C24 178.13(17) . . . . ? N6 C28 C29 C30 -1.4(3) . . . . ? N8 C37 C39 N7 -1.0(2) . . . . ? N8 C37 C39 C40 173.56(19) . . . . ? N9 C43 C44 C45 2.1(3) . . . . ? C17 P2 C28 N6 162.56(13) . . . . ? C17 P2 C28 C29 -25.20(17) . . . . ? C17 N4 C23 C21 -0.8(2) . . . . ? C17 N4 C23 C24 -178.59(17) . . . . ? C17 N4 C25 C26 123.22(18) . . . . ? C17 N4 C25 C27 -109.48(19) . . . . ? C17 N5 C18 C19 74.3(2) . . . . ? C17 N5 C18 C20 -57.6(2) . . . . ? C17 N5 C21 C22 176.02(18) . . . . ? C17 N5 C21 C23 0.1(2) . . . . ? C18 N5 C17 P2 -7.4(2) . . . . ? C18 N5 C17 N4 176.43(16) . . . . ? C18 N5 C21 C22 -1.3(3) . . . . ? C18 N5 C21 C23 -177.16(16) . . . . ? C21 N5 C17 P2 175.51(12) . . . . ? C21 N5 C17 N4 -0.65(19) . . . . ? C21 N5 C18 C19 -109.0(2) . . . . ? C21 N5 C18 C20 119.09(19) . . . . ? C22 C21 C23 N4 -175.20(19) . . . . ? C22 C21 C23 C24 2.5(3) . . . . ? C23 N4 C17 P2 -174.68(14) . . . . ? C23 N4 C17 N5 0.93(19) . . . . ? C23 N4 C25 C26 -58.4(2) . . . . ? C23 N4 C25 C27 68.9(2) . . . . ? C25 N4 C17 P2 3.9(3) . . . . ? C25 N4 C17 N5 179.53(15) . . . . ? C25 N4 C23 C21 -179.41(16) . . . . ? C25 N4 C23 C24 2.8(3) . . . . ? C28 P2 C17 N4 -55.50(18) . . . . ? C28 P2 C17 N5 129.40(14) . . . . ? C28 N6 C32 C31 -0.7(3) . . . . ? C28 C29 C30 C31 0.2(3) . . . . ? C29 C30 C31 C32 0.6(3) . . . . ? C30 C31 C32 N6 -0.4(3) . . . . ? C32 N6 C28 P2 173.83(15) . . . . ? C32 N6 C28 C29 1.6(3) . . . . ? C33 P3 C43 N9 -167.37(13) . . . . ? C33 P3 C43 C44 19.27(18) . . . . ? C33 N7 C39 C37 0.5(2) . . . . ? C33 N7 C39 C40 -174.46(18) . . . . ? C33 N7 C41A C029 -69.9(3) . . . . ? C33 N7 C41A C42A 58.9(3) . . . . ? C33 N7 C41B C029 -96.2(13) . . . . ? C33 N7 C41B C42B 119.5(17) . . . . ? C33 N8 C34 C35 107.26(19) . . . . ? C33 N8 C34 C36 -125.71(18) . . . . ? C33 N8 C37 C38 178.25(18) . . . . ? C33 N8 C37 C39 1.2(2) . . . . ? C34 N8 C33 P3 -2.1(3) . . . . ? C34 N8 C33 N7 -179.86(15) . . . . ? C34 N8 C37 C38 -2.8(3) . . . . ? C34 N8 C37 C39 -179.87(16) . . . . ? C37 N8 C33 P3 176.88(14) . . . . ? C37 N8 C33 N7 -0.86(19) . . . . ? C37 N8 C34 C35 -71.6(2) . . . . ? C37 N8 C34 C36 55.5(2) . . . . ? C38 C37 C39 N7 -178.01(18) . . . . ? C38 C37 C39 C40 -3.5(3) . . . . ? C39 N7 C33 P3 -177.81(13) . . . . ? C39 N7 C33 N8 0.2(2) . . . . ? C39 N7 C41A C029 110.3(2) . . . . ? C39 N7 C41A C42A -120.9(2) . . . . ? C39 N7 C41B C029 93.4(12) . . . . ? C39 N7 C41B C42B -51(2) . . . . ? C41A N7 C33 P3 2.4(3) . . . . ? C41A N7 C33 N8 -179.57(18) . . . . ? C41A N7 C39 C37 -179.69(17) . . . . ? C41A N7 C39 C40 5.4(3) . . . . ? C41B N7 C33 P3 9.3(7) . . . . ? C41B N7 C33 N8 -172.7(7) . . . . ? C41B N7 C39 C37 171.2(9) . . . . ? C41B N7 C39 C40 -3.7(10) . . . . ? C43 P3 C33 N7 -125.84(15) . . . . ? C43 P3 C33 N8 56.67(19) . . . . ? C43 N9 C47 C46 0.2(3) . . . . ? C43 C44 C45 C46 -1.0(3) . . . . ? C44 C45 C46 C47 -0.3(3) . . . . ? C45 C46 C47 N9 0.8(3) . . . . ? C47 N9 C43 P3 -175.04(14) . . . . ? C47 N9 C43 C44 -1.6(3) . . . . ? 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 -2.7556 12.4700 10.4611 -0.1790 0.9635 0.1990 1.0000 -0.0011 -5.0020 -0.0396 -0.3503 0.1159 -0.0002 -0.9993 -0.0002 0.0287 -0.0133 -0.0304 -1.5678 17.2326 9.0539 -0.4573 0.8398 0.2925 -0.8901 12.0186 12.4623 -0.4765 0.8762 -0.0714 0.0003 -2.0004 5.0005 -0.0471 0.2258 -0.2696 -1.0001 5.0006 -2.9984 0.0633 0.0129 0.3702 -2.0006 5.0032 -1.9972 0.1864 0.1613 0.4214 -5.0029 1.0142 -0.9950 0.7123 0.4521 0.5367 -1.0011 -4.9948 3.0004 0.2248 0.1828 -0.1844 0.9999 -4.9999 0.9980 -0.0215 -0.1139 -0.2867 1.0012 -0.0047 5.0000 -0.2484 0.1545 -0.3017 0.0007 4.9970 -0.9990 -0.1225 0.0160 0.1938 1.0007 -0.0033 0.9992 -0.1649 -0.0474 -0.1347 2.0021 4.9908 -0.0007 -0.4315 -0.1292 -0.0338 -2.0017 -4.9919 3.0014 0.3688 0.2806 -0.0915 5.0029 -1.0142 0.9950 -0.7123 -0.4521 -0.5367 -0.0001 0.0004 -1.0002 0.0209 -0.0505 0.0418 -0.0013 -4.9952 -4.0021 0.2270 -0.2685 0.0150 -0.0005 -4.9977 2.9994 0.0808 0.0849 -0.2773 -2.3891 9.3751 12.3744 -0.1830 0.9831 -0.0091