#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577316.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_1577316 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 'C51 H75 N6 P4, 3(C F3 O3 S), 4(C H2 Cl2)' _chemical_formula_sum 'C58 H83 Cl8 F9 N6 O9 P4 S3' _chemical_formula_weight 1682.96 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-02-20 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 74.3662(18) _cell_angle_beta 85.3052(17) _cell_angle_gamma 68.1297(18) _cell_formula_units_Z 2 _cell_length_a 14.3379(3) _cell_length_b 16.0023(3) _cell_length_c 19.1242(4) _cell_measurement_reflns_used 21139 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.2600 _cell_measurement_theta_min 3.0740 _cell_volume 3920.55(15) _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 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (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 0.982 _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 -52.00 -7.00 0.50 2.50 -- -38.50 -77.00 -90.00 90 2 \w -26.00 74.00 0.50 2.50 -- 42.50 -77.00-180.00 200 3 \w 84.00 109.00 0.50 10.00 -- 111.00 -94.00 -60.00 50 4 \w 100.00 127.00 0.50 10.00 -- 111.00 -61.00 0.00 54 5 \w 88.00 121.00 0.50 10.00 -- 111.00-125.00 90.00 66 6 \w 113.00 141.00 0.50 10.00 -- 111.00 -77.00 120.00 56 7 \w 57.00 84.00 0.50 10.00 -- 111.00 -94.00 30.00 54 8 \w 47.00 73.00 0.50 10.00 -- 111.00 -61.00 0.00 52 9 \w 41.00 70.00 0.50 10.00 -- 111.00-125.00 90.00 58 10 \w 39.00 96.00 0.50 10.00 -- 111.00 -77.00 120.00 114 11 \w 43.00 134.00 0.50 10.00 -- 111.00 -45.00 120.00 182 12 \w 89.00 173.00 0.50 10.00 -- 111.00 45.00 120.00 168 13 \w 106.00 139.00 0.50 10.00 -- 111.00 61.00 -30.00 66 14 \w 152.00 177.00 0.50 10.00 -- 111.00 61.00 -30.00 50 15 \w 108.00 135.00 0.50 10.00 -- 111.00 125.00 -90.00 54 16 \w 95.00 131.00 0.50 10.00 -- 111.00 125.00-150.00 72 17 \w 117.00 144.00 0.50 10.00 -- 111.00 125.00-180.00 54 18 \w 145.00 178.00 0.50 10.00 -- 111.00 125.00-180.00 66 19 \w 100.00 164.00 0.50 10.00 -- 111.00 30.00-120.00 128 20 \w 89.00 178.00 0.50 10.00 -- 111.00 30.00-180.00 178 21 \w 87.00 148.00 0.50 10.00 -- 111.00 45.00 30.00 122 22 \w 97.00 144.00 0.50 10.00 -- 111.00 125.00 60.00 94 23 \w 31.00 95.00 0.50 10.00 -- 111.00 -94.00 0.00 128 24 \w 51.00 78.00 0.50 10.00 -- 111.00-125.00 -60.00 54 25 \w 77.00 121.00 0.50 10.00 -- 111.00-125.00-120.00 88 26 \w 96.00 121.00 0.50 10.00 -- 111.00-125.00-150.00 50 27 \w 58.00 83.00 0.50 10.00 -- 111.00-125.00-150.00 50 28 \w 39.00 121.00 0.50 10.00 -- 111.00-123.00 -56.14 164 29 \w 43.00 119.00 0.50 10.00 -- 111.00-125.00 0.00 152 30 \w 33.00 107.00 0.50 10.00 -- 111.00 -94.00 90.00 148 31 \w 31.00 77.00 0.50 10.00 -- 111.00 -94.00 -60.00 92 32 \w -95.00 -10.00 0.50 2.50 -- -38.50 127.00 38.00 170 33 \w -106.00 -47.00 0.50 2.50 -- -38.50 -38.00 0.00 118 34 \w -107.00 -76.00 0.50 2.50 -- -38.50 -77.00 -90.00 62 35 \w -110.00 -16.00 0.50 2.50 -- -38.50 -38.00 -90.00 188 ; _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 -0.0011450000 _diffrn_orient_matrix_UB_12 0.0207268000 _diffrn_orient_matrix_UB_13 -0.0834705000 _diffrn_orient_matrix_UB_21 0.1069120000 _diffrn_orient_matrix_UB_22 0.0015908000 _diffrn_orient_matrix_UB_23 -0.0013422000 _diffrn_orient_matrix_UB_31 0.0444892000 _diffrn_orient_matrix_UB_32 -0.1053531000 _diffrn_orient_matrix_UB_33 0.0055949000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 42231 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.835 _diffrn_reflns_theta_min 2.400 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.789 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_correction_T_min 0.225 _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 1.426 _exptl_crystal_description plate _exptl_crystal_F_000 1740 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.335 _exptl_crystal_size_min 0.109 _refine_diff_density_max 0.823 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1178 _refine_ls_number_reflns 16256 _refine_ls_number_restraints 1069 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0642 _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^)+(0.1104P)^2^+4.0710P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1749 _refine_ls_wR_factor_ref 0.1817 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14524 _reflns_number_total 16256 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1043 _cod_original_cell_volume 3920.54(15) _cod_database_code 1577316 _chemical_oxdiff_formula 'C116 H150 Cl12 F18 N15 O18 P8 S6 ' _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 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 S3B \\sim F7B \\sim F9B \\sim O7B \\sim O8B \\sim O9B \\sim C54B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Cl3A \\sim Cl4A \\sim C56A \\sim Cl3B \\sim Cl4B \\sim C56B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 O5 \\sim O6 \\sim S2A \\sim F4A \\sim F5A \\sim F6A \\sim O4A \\sim C53A \\sim S2B \\sim F4B \\sim F5B \\sim F6B \\sim O4B \\sim C53B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 S3C \\sim F7C \\sim F8C \\sim F9C \\sim O7C \\sim O8C \\sim O9C \\sim C54C \\sim S3B \\sim F7B \\sim F8B \\sim F9B \\sim O7B \\sim O8B \\sim O9B \\sim C54B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 S3A \\sim F7A \\sim F8A \\sim F9A \\sim O7A \\sim O8A \\sim O9A \\sim C54A \\sim S3C \\sim F7C \\sim F8C \\sim F9C \\sim O7C \\sim O8C \\sim O9C \\sim C54C \\sim S3B \\sim F7B \\sim F8B \\sim F9B \\sim O7B \\sim O8B \\sim O9B \\sim C54B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Cl11 \\sim Cl12 \\sim C59B \\sim Cl9 \\sim Cl10 \\sim C59A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Cl7A \\sim Cl8A \\sim C58A \\sim Cl7B \\sim Cl8B \\sim C58B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Cl5B \\sim Cl6B \\sim C57B \\sim Cl5A \\sim Cl6A \\sim C57A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Same fragment restrains {S2B, F4B, F5B, F6B, O4B, C53B} sigma for 1-2: 0.02, 1-3: 0.02 as {S2A, F4A, F5A, F6A, O4A, C53A} {S3B, F7B, F8B, F9B, O9B, O7B, O8B, C54B} sigma for 1-2: 0.02, 1-3: 0.02 {S3C, F7C, F8C, F9C, O8C, O7C, O9C, C54C} sigma for 1-2: 0.02, 1-3: 0.02 as {S3A, F7A, F8A, F9A, O7A, O8A, O9A, C54A} {Cl8A, Cl7A, C58A} sigma for 1-2: 0.02, 1-3: 0.02 {Cl2, Cl1, C55} sigma for 1-2: 0.02, 1-3: 0.02 {Cl11, Cl12, C59B} sigma for 1-2: 0.02, 1-3: 0.02 {Cl9, Cl10, C59A} sigma for 1-2: 0.02, 1-3: 0.02 {Cl6B, Cl5B, C57B} sigma for 1-2: 0.02, 1-3: 0.02 {Cl5A, Cl6A, C57A} sigma for 1-2: 0.02, 1-3: 0.02 {Cl4B, Cl3B, C56B} sigma for 1-2: 0.02, 1-3: 0.02 {Cl3A, Cl4A, C56A} sigma for 1-2: 0.02, 1-3: 0.02 as {Cl7B, Cl8B, C58B} 4. Others 1*[Sof(S3A)+Sof(F7A)+Sof(F8A)+Sof(F9A)+Sof(O7A)+Sof(O8A)+Sof(O9A)+Sof(C54A)]+ 1*[Sof(S3B)+Sof(F7B)+Sof(F8B)+Sof(F9B)+Sof(O9B)+Sof(O7B)+Sof(O8B)+Sof(C54B)]+1* [Sof(S3C)+Sof(F7C)+Sof(F8C)+Sof(F9C)+Sof(O8C)+Sof(O7C)+Sof(O9C)+Sof(C54C)]=1 with esd of 0 Sof(S3A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(C54A)= FVAR(1) Sof(Cl4B)=Sof(Cl3B)=Sof(C56B)=Sof(H56C)=Sof(H56D)=1-FVAR(2) Sof(Cl3A)=Sof(Cl4A)=Sof(C56A)=Sof(H56A)=Sof(H56B)=FVAR(2) Sof(S2B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O4B)=Sof(C53B)=1-FVAR(3) Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(C53A)=FVAR(3) Sof(S3B)=Sof(F7B)=Sof(F8B)=Sof(F9B)=Sof(O9B)=Sof(O7B)=Sof(O8B)=Sof(C54B)= FVAR(4) Sof(S3C)=Sof(F7C)=Sof(F8C)=Sof(F9C)=Sof(O8C)=Sof(O7C)=Sof(O9C)=Sof(C54C)= FVAR(5) Sof(Cl11)=Sof(Cl12)=Sof(C59B)=Sof(H59A)=Sof(H59B)=1-FVAR(6) Sof(Cl9)=Sof(Cl10)=Sof(C59A)=Sof(H59C)=Sof(H59D)=FVAR(6) Sof(Cl6B)=Sof(Cl5B)=Sof(C57B)=Sof(H57A)=Sof(H57B)=0.5*(1-FVAR(8)) Sof(Cl5A)=Sof(Cl6A)=Sof(C57A)=Sof(H57C)=Sof(H57D)=0.5*FVAR(8) Sof(Cl8A)=Sof(Cl7A)=Sof(C58A)=Sof(H58A)=Sof(H58B)=0.5*(1-FVAR(9)) Sof(Cl7B)=Sof(Cl8B)=Sof(C58B)=Sof(H58C)=Sof(H58D)=0.5*FVAR(9) 5.a Ternary CH refined with riding coordinates: C4(H4), C7(H7), C21(H21), C24(H24), C38(H38), C41(H41) 5.b Secondary CH2 refined with riding coordinates: C59B(H59A,H59B), C56A(H56A,H56B), C59A(H59C,H59D), C57B(H57A,H57B), C55(H55A, H55B), C58A(H58A,H58B), C57A(H57C,H57D), C56B(H56C,H56D), C58B(H58C,H58D) 5.c Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51) 5.d Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B, H28C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A, H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C) ; _shelx_res_file ; jjw1043.res created by SHELXL-2014/7 TITL jjw1043_a.res in P-1 REM Old TITL jjw1043 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.191, Rweak 0.011, Alpha 0.059, Orientation as input REM Formula found by SHELXT: C125 N16 O14 F18 P4 S4 Cl5A CELL 1.54184 14.337851 16.002299 19.124168 74.3662 85.3052 68.1297 ZERR 2 0.000282 0.000296 0.000421 0.0018 0.0017 0.0018 LATT 1 SFAC C H Cl F N O P S UNIT 116 166 16 18 12 18 8 6 SIMU 0.01 0.02 2 S3B F7B F9B O7B O8B O9B C54B SIMU 0.01 0.02 2 Cl3A Cl4A C56A Cl3B Cl4B C56B SIMU 0.01 0.02 2 O5 > C53B SIMU 0.01 0.02 2 S3C > F9C O7C O8C O9C > F9B O7B O8B O9B C54B SIMU 0.01 0.02 2 S3A > C54A S3C > F9C O7C O8C O9C > F9B O7B O8B O9B C54B SIMU 0.01 0.02 2 Cl11 Cl12 C59B Cl9 > C59A SIMU 0.01 0.02 2 Cl7A Cl8A C58A Cl7B > C58B SIMU 0.01 0.02 2 Cl5B Cl6B C57B Cl5A > C57A SUMP 1 0 1 2 1 5 1 6 L.S. 10 PLAN 40 BOND $H LIST 6 MORE -1 CONF fmap 2 TEMP 100 ACTA OMIT 1 -1 2 OMIT 1 -1 1 REM REM REM WGHT 0.110400 4.071000 FVAR 0.30470 0.63377 0.74532 0.75907 0.25102 0.11519 0.85001 FVAR 0.52728 0.59227 P1 7 0.183696 0.621814 0.260458 11.00000 0.02076 0.02398 = 0.01889 -0.00214 -0.00260 -0.01179 P2 7 0.287862 0.642797 0.168141 11.00000 0.02061 0.02649 = 0.01805 -0.00149 -0.00328 -0.01274 P3 7 0.055621 0.736833 0.190526 11.00000 0.02104 0.02493 = 0.02319 0.00075 -0.00278 -0.01131 P4 7 0.153636 0.518469 0.213931 11.00000 0.02389 0.02559 = 0.01863 -0.00353 -0.00016 -0.01368 N1 5 0.325029 0.791272 0.209377 11.00000 0.02468 0.02672 = 0.02033 -0.00102 -0.00237 -0.01465 N2 5 0.246713 0.831548 0.104982 11.00000 0.02066 0.02839 = 0.02099 -0.00005 -0.00239 -0.01007 N3 5 -0.094210 0.702115 0.294825 11.00000 0.01875 0.02744 = 0.02372 0.00246 -0.00490 -0.00966 N4 5 -0.098732 0.670725 0.190896 11.00000 0.02463 0.02745 = 0.02707 0.00050 -0.00980 -0.01195 N5 5 0.336587 0.363591 0.278209 11.00000 0.02433 0.02623 = 0.03032 -0.00990 0.00234 -0.01070 N6 5 0.329780 0.412034 0.159366 11.00000 0.02985 0.03983 = 0.02585 -0.01335 0.00460 -0.01906 C1 1 0.285916 0.759329 0.164153 11.00000 0.02090 0.02720 = 0.01857 -0.00003 -0.00285 -0.01310 C2 1 0.310990 0.883702 0.177769 11.00000 0.02986 0.02656 = 0.02861 -0.00380 0.00022 -0.01407 C3 1 0.261025 0.909189 0.113040 11.00000 0.02686 0.02582 = 0.02822 -0.00095 0.00064 -0.01132 C4 1 0.377065 0.732231 0.280449 11.00000 0.02936 0.03186 = 0.02103 -0.00085 -0.00662 -0.01792 AFIX 13 H4 2 0.360308 0.675992 0.293089 11.00000 -1.20000 AFIX 0 C5 1 0.343004 0.778613 0.342979 11.00000 0.04314 0.04269 = 0.02474 -0.00603 -0.00614 -0.02448 AFIX 137 H5A 2 0.372012 0.825039 0.338367 11.00000 -1.50000 H5B 2 0.364551 0.732456 0.388323 11.00000 -1.50000 H5C 2 0.271037 0.807500 0.341555 11.00000 -1.50000 AFIX 0 C6 1 0.490551 0.700909 0.272137 11.00000 0.02832 0.03464 = 0.03278 -0.00078 -0.00877 -0.01734 AFIX 137 H6A 2 0.509626 0.673413 0.231819 11.00000 -1.50000 H6B 2 0.523090 0.655821 0.315716 11.00000 -1.50000 H6C 2 0.510510 0.753741 0.263633 11.00000 -1.50000 AFIX 0 C7 1 0.206273 0.822204 0.039115 11.00000 0.02723 0.03526 = 0.01909 0.00136 -0.00699 -0.01197 AFIX 13 H7 2 0.194895 0.763226 0.052897 11.00000 -1.20000 AFIX 0 C8 1 0.285260 0.814543 -0.019619 11.00000 0.03695 0.05171 = 0.02496 -0.00588 -0.00209 -0.01501 AFIX 137 H8A 2 0.298919 0.871077 -0.034164 11.00000 -1.50000 H8B 2 0.260717 0.804703 -0.060777 11.00000 -1.50000 H8C 2 0.345907 0.763024 -0.000920 11.00000 -1.50000 AFIX 0 C9 1 0.105618 0.899383 0.012599 11.00000 0.02880 0.04610 = 0.02935 0.00365 -0.01219 -0.00735 AFIX 137 H9A 2 0.066501 0.915184 0.053569 11.00000 -1.50000 H9B 2 0.070087 0.878293 -0.015059 11.00000 -1.50000 H9C 2 0.116821 0.953321 -0.017428 11.00000 -1.50000 AFIX 0 C10 1 0.348497 0.941150 0.209599 11.00000 0.04688 0.03031 = 0.03789 -0.00408 -0.00446 -0.02205 AFIX 137 H10A 2 0.305761 0.959643 0.248370 11.00000 -1.50000 H10B 2 0.348010 0.995615 0.172746 11.00000 -1.50000 H10C 2 0.415840 0.905136 0.228150 11.00000 -1.50000 AFIX 0 C11 1 0.225323 1.003723 0.060453 11.00000 0.04103 0.02835 = 0.03383 0.00345 -0.00267 -0.01278 AFIX 137 H11A 2 0.240917 0.997357 0.011927 11.00000 -1.50000 H11B 2 0.258248 1.041158 0.071503 11.00000 -1.50000 H11C 2 0.153951 1.033165 0.064268 11.00000 -1.50000 AFIX 0 C12 1 0.415775 0.567594 0.200347 11.00000 0.02311 0.02648 = 0.02105 -0.00259 -0.00343 -0.01375 C13 1 0.443222 0.510986 0.270623 11.00000 0.02686 0.02868 = 0.02069 -0.00236 -0.00314 -0.01468 AFIX 43 H13 2 0.395063 0.512025 0.306377 11.00000 -1.20000 AFIX 0 C14 1 0.543342 0.452822 0.286924 11.00000 0.03034 0.02989 = 0.02580 0.00100 -0.00967 -0.01374 AFIX 43 H14 2 0.561522 0.414291 0.333539 11.00000 -1.20000 AFIX 0 C15 1 0.615678 0.451861 0.234612 11.00000 0.02304 0.03576 = 0.03528 -0.00482 -0.00890 -0.00940 AFIX 43 H15 2 0.682367 0.413488 0.246303 11.00000 -1.20000 AFIX 0 C16 1 0.589109 0.508116 0.164475 11.00000 0.02461 0.04185 = 0.02828 -0.00921 0.00042 -0.01422 AFIX 43 H16 2 0.637978 0.507842 0.129332 11.00000 -1.20000 AFIX 0 C17 1 0.489782 0.564467 0.147158 11.00000 0.02483 0.03449 = 0.02096 -0.00249 -0.00258 -0.01387 AFIX 43 H17 2 0.471764 0.600655 0.099855 11.00000 -1.20000 AFIX 0 C18 1 -0.049421 0.701706 0.229700 11.00000 0.01936 0.02353 = 0.02402 0.00082 -0.00583 -0.00917 C19 1 -0.173700 0.672597 0.296578 11.00000 0.02013 0.03358 = 0.03255 0.00616 -0.00786 -0.01230 C20 1 -0.175657 0.652062 0.232146 11.00000 0.02273 0.03126 = 0.03658 0.00401 -0.00919 -0.01381 C21 1 -0.066001 0.737531 0.351267 11.00000 0.02422 0.03059 = 0.02582 -0.00334 -0.00480 -0.00834 AFIX 13 H21 2 0.000983 0.739552 0.339043 11.00000 -1.20000 AFIX 0 C22 1 -0.135564 0.836919 0.347381 11.00000 0.03866 0.03232 = 0.03697 -0.00511 -0.00285 -0.00574 AFIX 137 H22A 2 -0.140599 0.874025 0.298167 11.00000 -1.50000 H22B 2 -0.109177 0.861993 0.377950 11.00000 -1.50000 H22C 2 -0.200985 0.837701 0.363566 11.00000 -1.50000 AFIX 0 C23 1 -0.057126 0.674662 0.428484 11.00000 0.03109 0.03552 = 0.02316 -0.00323 -0.00191 -0.00658 AFIX 137 H23A 2 -0.123091 0.680801 0.446768 11.00000 -1.50000 H23B 2 -0.022548 0.692750 0.459229 11.00000 -1.50000 H23C 2 -0.020174 0.611012 0.427878 11.00000 -1.50000 AFIX 0 C24 1 -0.080616 0.671699 0.112521 11.00000 0.03519 0.03554 = 0.02734 -0.00469 -0.01175 -0.01209 AFIX 13 H24 2 -0.015408 0.678293 0.101148 11.00000 -1.20000 AFIX 0 C25 1 -0.159001 0.757670 0.065444 11.00000 0.05005 0.04687 = 0.02996 0.00174 -0.01307 -0.00426 AFIX 137 H25A 2 -0.224668 0.755408 0.076595 11.00000 -1.50000 H25B 2 -0.145823 0.759276 0.015161 11.00000 -1.50000 H25C 2 -0.155998 0.812598 0.074855 11.00000 -1.50000 AFIX 0 C26 1 -0.073070 0.581759 0.095935 11.00000 0.05910 0.04238 = 0.04288 -0.01113 -0.02203 -0.01788 AFIX 137 H26A 2 -0.033999 0.529538 0.133492 11.00000 -1.50000 H26B 2 -0.041201 0.578242 0.050118 11.00000 -1.50000 H26C 2 -0.139241 0.580664 0.093716 11.00000 -1.50000 AFIX 0 C27 1 -0.244148 0.668224 0.358259 11.00000 0.02565 0.05642 = 0.03961 0.00622 -0.00094 -0.02003 AFIX 137 H27A 2 -0.212284 0.613964 0.396851 11.00000 -1.50000 H27B 2 -0.303944 0.664838 0.342027 11.00000 -1.50000 H27C 2 -0.261506 0.723059 0.375556 11.00000 -1.50000 AFIX 0 C28 1 -0.246281 0.614618 0.209748 11.00000 0.03142 0.04845 = 0.05734 -0.00358 -0.01486 -0.02403 AFIX 137 H28A 2 -0.279225 0.654823 0.164668 11.00000 -1.50000 H28B 2 -0.295633 0.611704 0.246468 11.00000 -1.50000 H28C 2 -0.209396 0.553251 0.203708 11.00000 -1.50000 AFIX 0 C29 1 0.037153 0.841248 0.220574 11.00000 0.02542 0.02592 = 0.03955 -0.00291 0.00049 -0.01342 C30 1 0.092546 0.844435 0.274990 11.00000 0.03180 0.03023 = 0.05623 -0.01055 -0.00600 -0.01385 AFIX 43 H30 2 0.140624 0.790144 0.301834 11.00000 -1.20000 AFIX 0 C31 1 0.075597 0.930042 0.289275 11.00000 0.04639 0.04051 = 0.08870 -0.02651 -0.01160 -0.01797 AFIX 43 H31 2 0.112579 0.932671 0.325833 11.00000 -1.20000 AFIX 0 C32 1 0.004282 1.010758 0.249450 11.00000 0.05382 0.03037 = 0.09700 -0.02102 -0.00376 -0.01735 AFIX 43 H32 2 -0.006473 1.067415 0.259332 11.00000 -1.20000 AFIX 0 C33 1 -0.050957 1.007797 0.195215 11.00000 0.04262 0.02713 = 0.06793 -0.00199 0.00037 -0.00986 AFIX 43 H33 2 -0.099268 1.062260 0.168792 11.00000 -1.20000 AFIX 0 C34 1 -0.034504 0.923652 0.180058 11.00000 0.03442 0.02887 = 0.04396 0.00210 -0.00165 -0.01210 AFIX 43 H34 2 -0.071073 0.921772 0.142906 11.00000 -1.20000 AFIX 0 C35 1 0.279219 0.427152 0.220790 11.00000 0.02414 0.02713 = 0.02577 -0.00806 0.00211 -0.01288 C36 1 0.423638 0.307819 0.252171 11.00000 0.02318 0.03538 = 0.04489 -0.02018 0.00153 -0.00884 C37 1 0.419088 0.338666 0.178175 11.00000 0.02728 0.04565 = 0.03996 -0.02336 0.00617 -0.01613 C38 1 0.303861 0.353446 0.355735 11.00000 0.02581 0.02554 = 0.02588 -0.00156 0.00037 -0.00858 AFIX 13 H38 2 0.248530 0.411700 0.357413 11.00000 -1.20000 AFIX 0 C39 1 0.261027 0.275988 0.378066 11.00000 0.03290 0.02979 = 0.04375 0.00302 -0.00187 -0.01246 AFIX 137 H39A 2 0.204486 0.291206 0.347074 11.00000 -1.50000 H39B 2 0.239903 0.269835 0.427537 11.00000 -1.50000 H39C 2 0.311782 0.218258 0.373619 11.00000 -1.50000 AFIX 0 C40 1 0.384309 0.339377 0.409483 11.00000 0.03276 0.02892 = 0.02577 0.00035 -0.00247 -0.00981 AFIX 137 H40A 2 0.430310 0.275816 0.420101 11.00000 -1.50000 H40B 2 0.353245 0.353368 0.453457 11.00000 -1.50000 H40C 2 0.420147 0.380069 0.388812 11.00000 -1.50000 AFIX 0 C41 1 0.285806 0.464265 0.083954 11.00000 0.03653 0.04877 = 0.02277 -0.01408 0.00494 -0.02378 AFIX 13 H41 2 0.231020 0.521449 0.088718 11.00000 -1.20000 AFIX 0 C42 1 0.238344 0.408800 0.055603 11.00000 0.04811 0.05684 = 0.03719 -0.01911 -0.00079 -0.02997 AFIX 137 H42A 2 0.288635 0.349733 0.053648 11.00000 -1.50000 H42B 2 0.210433 0.442822 0.007800 11.00000 -1.50000 H42C 2 0.186015 0.398844 0.087471 11.00000 -1.50000 AFIX 0 C43 1 0.359770 0.494530 0.031398 11.00000 0.04810 0.06830 = 0.02888 -0.01852 0.00889 -0.03441 AFIX 137 H43A 2 0.401178 0.512813 0.056556 11.00000 -1.50000 H43B 2 0.323429 0.546274 -0.007550 11.00000 -1.50000 H43C 2 0.401369 0.443598 0.012030 11.00000 -1.50000 AFIX 0 C44 1 0.505620 0.229880 0.298097 11.00000 0.03070 0.04121 = 0.05408 -0.02172 -0.00388 -0.00131 AFIX 137 H44A 2 0.534604 0.253645 0.328124 11.00000 -1.50000 H44B 2 0.556355 0.199719 0.267654 11.00000 -1.50000 H44C 2 0.479023 0.185772 0.328272 11.00000 -1.50000 AFIX 0 C45 1 0.496280 0.302532 0.124943 11.00000 0.03459 0.06779 = 0.05093 -0.03546 0.01072 -0.01568 AFIX 137 H45A 2 0.464466 0.292272 0.087461 11.00000 -1.50000 H45B 2 0.546775 0.244878 0.149612 11.00000 -1.50000 H45C 2 0.526984 0.347329 0.103700 11.00000 -1.50000 AFIX 0 C46 1 0.081876 0.464782 0.282241 11.00000 0.02053 0.02332 = 0.02386 -0.00167 -0.00074 -0.01030 C47 1 0.056289 0.484114 0.349754 11.00000 0.02556 0.02576 = 0.02230 -0.00218 -0.00121 -0.01018 AFIX 43 H47 2 0.081435 0.522561 0.364580 11.00000 -1.20000 AFIX 0 C48 1 -0.006726 0.445940 0.394804 11.00000 0.02736 0.02873 = 0.02532 -0.00081 0.00270 -0.00932 AFIX 43 H48 2 -0.024471 0.459978 0.439317 11.00000 -1.20000 AFIX 0 C49 1 -0.043348 0.387253 0.374118 11.00000 0.02626 0.03012 = 0.03743 0.00139 0.00323 -0.01317 AFIX 43 H49 2 -0.084551 0.361184 0.404962 11.00000 -1.20000 AFIX 0 C50 1 -0.018278 0.367375 0.306945 11.00000 0.03016 0.03148 = 0.04153 -0.00495 -0.00065 -0.01918 AFIX 43 H50 2 -0.042412 0.327701 0.292946 11.00000 -1.20000 AFIX 0 C51 1 0.042982 0.407002 0.260781 11.00000 0.02927 0.03068 = 0.03042 -0.00780 0.00033 -0.01539 AFIX 43 H51 2 0.058157 0.395010 0.215406 11.00000 -1.20000 AFIX 0 O5 6 0.768772 -0.120588 0.187334 11.00000 0.03173 0.04258 = 0.04546 -0.01064 -0.01030 -0.00418 O6 6 0.639749 -0.025652 0.096549 11.00000 0.05818 0.05733 = 0.03920 -0.00458 -0.01545 0.00281 SAME 0.02 0.02 S2B > C53B PART 1 S2A 8 0.664973 -0.077234 0.171158 41.00000 0.02757 0.03044 = 0.03279 0.00144 -0.00892 -0.01418 F4A 4 0.524560 0.064628 0.207986 41.00000 0.03032 0.06829 = 0.05656 -0.02381 -0.01043 0.00660 F5A 4 0.645446 -0.010009 0.285589 41.00000 0.05175 0.08527 = 0.03212 -0.01629 -0.01267 0.00580 F6A 4 0.670751 0.076643 0.189225 41.00000 0.06050 0.04779 = 0.07081 -0.02560 0.00429 -0.02139 O4A 6 0.608907 -0.133894 0.206468 41.00000 0.05539 0.05652 = 0.10952 0.00606 -0.00352 -0.03809 C53A 1 0.622474 0.016273 0.216204 41.00000 0.02921 0.05365 = 0.03076 -0.00934 -0.00924 -0.00719 PART 0 PART 2 S2B 8 0.659762 -0.078108 0.165050 -41.00000 0.02795 0.03821 = 0.04526 -0.00776 -0.01143 -0.01059 F4B 4 0.511161 0.038946 0.221229 -41.00000 0.03670 0.05615 = 0.07693 -0.02439 -0.01531 -0.00257 F5B 4 0.611995 -0.067291 0.298741 -41.00000 0.06827 0.09563 = 0.03172 -0.01114 -0.00233 0.02389 F6B 4 0.662178 0.037769 0.234835 -41.00000 0.05087 0.06850 = 0.08699 -0.03849 -0.00830 -0.00694 O4B 6 0.603378 -0.135789 0.173618 -41.00000 0.04314 0.06860 = 0.08280 -0.03470 0.00529 -0.03919 C53B 1 0.607192 -0.017428 0.235272 -41.00000 0.03684 0.05357 = 0.05083 -0.01068 -0.01358 -0.00165 SAME 0.02 0.02 S3B > C54B SAME 0.02 0.02 S3C > C54C PART 0 PART 1 S3A 8 0.951705 0.293259 0.074508 21.00000 0.03073 0.03303 = 0.03664 -0.00682 -0.00057 -0.01126 F7A 4 0.778563 0.290621 0.132122 21.00000 0.04113 0.07739 = 0.06511 -0.02758 0.00637 -0.03592 F8A 4 0.895820 0.263330 0.209885 21.00000 0.06079 0.06607 = 0.03334 -0.01173 0.00017 -0.02873 F9A 4 0.818398 0.402789 0.144246 21.00000 0.03519 0.04769 = 0.06497 -0.02960 0.01116 -0.00716 O7A 6 1.016642 0.336475 0.089569 21.00000 0.02489 0.03665 = 0.05905 -0.00563 -0.00557 -0.01239 O8A 6 0.996539 0.194546 0.087874 21.00000 0.04452 0.03084 = 0.05186 -0.01675 0.00109 -0.00338 O9A 6 0.896346 0.338993 0.006324 21.00000 0.05528 0.06305 = 0.02874 -0.00316 -0.00024 -0.01592 C54A 1 0.859244 0.309973 0.144138 21.00000 0.02003 0.03152 = 0.01418 -0.01255 0.00851 -0.01703 PART 0 S1 8 0.249257 0.577225 0.463502 11.00000 0.02310 0.03527 = 0.02024 -0.00250 -0.00375 -0.01205 F1 4 0.387289 0.591839 0.535901 11.00000 0.04599 0.07852 = 0.03530 -0.01035 -0.00473 -0.04078 F2 4 0.284690 0.537107 0.604475 11.00000 0.04370 0.07911 = 0.02148 -0.01183 0.00362 -0.03029 F3 4 0.398802 0.450401 0.547938 11.00000 0.03115 0.05823 = 0.03443 0.00138 -0.00997 -0.00654 O1 6 0.185437 0.669982 0.466070 11.00000 0.03222 0.04052 = 0.04785 -0.00892 -0.00304 -0.01088 O2 6 0.199771 0.510678 0.477082 11.00000 0.02856 0.04127 = 0.03268 -0.00403 -0.00414 -0.01756 O3 6 0.319398 0.571826 0.404662 11.00000 0.03378 0.04888 = 0.02057 -0.00423 0.00105 -0.01840 C52 1 0.334274 0.537041 0.541781 11.00000 0.02889 0.05193 = 0.02265 -0.00587 -0.00045 -0.01995 PART 3 S3C 8 0.897556 0.368082 0.078693 61.00000 0.04478 F7C 4 0.816091 0.244913 0.147840 61.00000 0.05857 F8C 4 0.972524 0.187693 0.116954 61.00000 0.06575 F9C 4 0.933476 0.250490 0.206794 61.00000 0.05801 O8C 6 0.880116 0.362135 0.007894 61.00000 0.05404 O7C 6 0.999484 0.363064 0.088394 61.00000 0.04254 O9C 6 0.821886 0.442419 0.102536 61.00000 0.05231 C54C 1 0.901101 0.260758 0.138953 61.00000 0.05116 PART 0 PART 2 S3B 8 0.865772 0.318899 0.101307 51.00000 0.04005 0.04939 = 0.07570 -0.01593 0.00650 -0.01289 F7B 4 1.005069 0.236824 0.202886 51.00000 0.07479 0.06623 = 0.05355 -0.01042 0.00881 -0.01771 F8B 4 1.038064 0.180617 0.107710 51.00000 0.05984 0.05104 = 0.06661 -0.01688 0.00281 -0.00700 F9B 4 1.048154 0.313801 0.103505 51.00000 0.03727 0.04746 = 0.05214 -0.00680 0.00075 -0.01325 O9B 6 0.834558 0.405135 0.120694 51.00000 0.04303 0.04251 = 0.05450 -0.01640 0.02057 -0.00823 O7B 6 0.875107 0.331156 0.022587 51.00000 0.04911 0.05706 = 0.03652 -0.00350 -0.00782 -0.01283 O8B 6 0.815707 0.255548 0.134164 51.00000 0.04867 0.05592 = 0.07022 -0.00065 0.00402 -0.02530 C54B 1 0.994388 0.260241 0.130175 51.00000 0.04011 0.04166 = 0.04337 -0.00011 0.01000 0.00137 CL11 3 0.763239 0.080128 0.349993 -71.00000 0.11779 CL12 3 0.848895 0.201853 0.376188 -71.00000 0.15616 C59B 1 0.740676 0.177903 0.379905 -71.00000 0.13278 AFIX 23 H59A 2 0.717432 0.167964 0.429455 -71.00000 -1.20000 H59B 2 0.688478 0.230550 0.349788 -71.00000 -1.20000 AFIX 0 PART 0 PART 1 CL3A 3 0.276645 0.197833 0.203177 31.00000 0.04821 0.04482 = 0.04941 -0.01235 0.00577 -0.01962 CL4A 3 0.152786 0.121671 0.306905 31.00000 0.08234 0.07434 = 0.09204 -0.04385 0.03632 -0.05779 C56A 1 0.166291 0.172443 0.216366 31.00000 0.04644 0.05196 = 0.08941 -0.03596 -0.00809 -0.01458 AFIX 23 H56A 2 0.108626 0.229485 0.199996 31.00000 -1.20000 H56B 2 0.168367 0.130438 0.187462 31.00000 -1.20000 AFIX 0 CL9 3 0.786824 0.229145 0.362770 71.00000 0.08566 0.06668 = 0.10576 0.00992 -0.01798 -0.02967 CL10 3 0.673824 0.152979 0.474917 71.00000 0.19074 0.13164 = 0.07805 -0.01093 0.00560 -0.09143 C59A 1 0.776096 0.187183 0.454791 71.00000 0.13953 0.07040 = 0.09336 -0.01472 -0.01683 -0.03697 AFIX 23 H59C 2 0.769427 0.235263 0.478823 71.00000 -1.20000 H59D 2 0.836903 0.134418 0.473505 71.00000 -1.20000 AFIX 0 PART 0 PART -2 CL6B 3 -0.040139 -0.041657 0.549297 -80.50000 0.26036 0.16763 = 0.14162 -0.02270 -0.01958 -0.10814 CL5B 3 0.042700 0.103402 0.492904 -80.50000 0.24398 0.19026 = 0.15532 -0.07065 0.01401 -0.13327 C57B 1 -0.065422 0.076925 0.509179 -80.50000 0.26343 0.15643 = 0.13881 -0.03738 -0.00204 -0.10811 AFIX 23 H57A 2 -0.101734 0.095043 0.463588 -80.50000 -1.20000 H57B 2 -0.108397 0.113052 0.540773 -80.50000 -1.20000 AFIX 0 PART 0 CL2 3 0.396377 0.140422 0.051505 11.00000 0.04115 0.05075 = 0.03825 0.00054 -0.00280 -0.02131 CL1 3 0.477353 0.235228 -0.074607 11.00000 0.04070 0.04367 = 0.04886 0.01281 -0.01015 -0.02142 C55 1 0.477874 0.126047 -0.021576 11.00000 0.03757 0.03474 = 0.03967 0.00077 -0.00666 -0.01440 AFIX 23 H55A 2 0.456855 0.095636 -0.051434 11.00000 -1.20000 H55B 2 0.545496 0.086652 -0.003306 11.00000 -1.20000 AFIX 0 PART -1 CL8A 3 0.471891 0.119854 0.599950 -90.50000 0.10738 0.14215 = 0.11490 -0.03015 0.01628 -0.06553 CL7A 3 0.467498 0.049552 0.479327 -90.50000 0.18664 0.13659 = 0.15388 0.00859 0.00165 0.00162 C58A 1 0.500838 0.025665 0.567220 -90.50000 0.10847 0.09120 = 0.10460 -0.00910 0.00976 -0.02840 AFIX 23 H58A 2 0.468141 -0.014839 0.596474 -90.50000 -1.20000 H58B 2 0.572821 -0.008362 0.572673 -90.50000 -1.20000 AFIX 0 CL5A 3 0.098931 0.109866 0.472686 80.50000 0.29962 0.17032 = 0.17158 -0.04630 0.01204 -0.14825 CL6A 3 -0.025327 -0.000500 0.506162 80.50000 0.25432 0.10041 = 0.09408 -0.00686 -0.02167 -0.09585 C57A 1 0.047024 0.047330 0.540079 80.50000 0.25670 0.14103 = 0.13390 -0.04121 -0.00157 -0.12890 AFIX 23 H57C 2 0.005088 0.087689 0.569291 80.50000 -1.20000 H57D 2 0.100297 -0.002505 0.571347 80.50000 -1.20000 AFIX 0 PART 0 PART 2 CL4B 3 0.261933 0.192610 0.220961 -31.00000 0.11434 0.11149 = 0.16029 -0.06462 0.02607 -0.03813 CL3B 3 0.274667 0.050853 0.355633 -31.00000 0.23755 0.13657 = 0.16868 -0.06925 0.01740 -0.03731 C56B 1 0.201917 0.138030 0.286640 -31.00000 0.08948 0.08160 = 0.12247 -0.03817 0.01920 -0.03404 AFIX 23 H56C 2 0.165168 0.112094 0.263715 -31.00000 -1.20000 H56D 2 0.152809 0.184647 0.307807 -31.00000 -1.20000 AFIX 0 SAME 0.02 0.02 Cl8A Cl7A C58A SAME 0.02 0.02 Cl2 Cl1 C55 SAME 0.02 0.02 Cl11 Cl12 C59B SAME 0.02 0.02 Cl9 Cl10 C59A SAME 0.02 0.02 Cl6B Cl5B C57B SAME 0.02 0.02 Cl5A Cl6A C57A SAME 0.02 0.02 Cl4B Cl3B C56B SAME 0.02 0.02 Cl3A Cl4A C56A PART 0 PART 3 CL7B 3 0.586819 -0.001178 0.627903 90.50000 0.04978 0.05287 = 0.05635 -0.00914 -0.00612 -0.01577 CL8B 3 0.401188 0.101660 0.544251 90.50000 0.06573 0.07975 = 0.04618 -0.00244 -0.01246 -0.02849 C58B 1 0.529259 0.048649 0.542036 90.50000 0.11701 0.09041 = 0.11344 -0.01362 -0.00092 -0.02047 AFIX 23 H58C 2 0.557006 0.094355 0.514904 90.50000 -1.20000 H58D 2 0.545031 0.000502 0.516395 90.50000 -1.20000 AFIX 0 HKLF 4 REM jjw1043_a.res in P-1 REM R1 = 0.0642 for 14524 Fo > 4sig(Fo) and 0.0696 for all 16256 data REM 1178 parameters refined using 1069 restraints END WGHT 0.1104 4.0707 REM Highest difference peak 0.823, deepest hole -0.880, 1-sigma level 0.093 Q1 1 0.2147 0.0802 0.3251 11.00000 0.05 0.82 Q2 1 0.6589 0.0168 0.1169 11.00000 0.05 0.77 Q3 1 0.6363 0.2021 0.4677 11.00000 0.05 0.77 Q4 1 0.3831 0.0240 0.5402 11.00000 0.05 0.75 Q5 1 0.5375 0.0665 0.5016 11.00000 0.05 0.73 Q6 1 0.5320 0.0504 0.5874 11.00000 0.05 0.72 Q7 1 0.7230 0.1360 0.4978 11.00000 0.05 0.68 Q8 1 0.3558 0.1804 0.0717 11.00000 0.05 0.66 Q9 1 0.4405 0.2283 -0.0405 11.00000 0.05 0.66 Q10 1 0.6805 -0.0130 0.1776 11.00000 0.05 0.59 Q11 1 0.6745 0.1177 0.4463 11.00000 0.05 0.57 Q12 1 0.2155 0.4729 0.2284 11.00000 0.05 0.57 Q13 1 0.4210 0.1529 0.5709 11.00000 0.05 0.56 Q14 1 0.4780 0.0477 0.5455 11.00000 0.05 0.53 Q15 1 0.5841 -0.0799 0.1408 11.00000 0.05 0.52 Q16 1 0.7994 0.2148 0.4198 11.00000 0.05 0.52 Q17 1 0.5930 -0.0553 0.1280 11.00000 0.05 0.50 Q18 1 0.0126 0.1338 0.4344 11.00000 0.05 0.50 Q19 1 0.8068 0.2182 0.3154 11.00000 0.05 0.49 Q20 1 0.4998 0.0775 0.6054 11.00000 0.05 0.48 Q21 1 0.4097 0.4472 0.0462 11.00000 0.05 0.47 Q22 1 0.5781 -0.0983 0.2882 11.00000 0.05 0.47 Q23 1 0.8194 0.1939 0.4290 11.00000 0.05 0.46 Q24 1 0.4330 0.3098 0.2127 11.00000 0.05 0.46 Q25 1 0.8487 0.3559 0.0656 11.00000 0.05 0.44 Q26 1 0.7414 0.2285 0.4100 11.00000 0.05 0.44 Q27 1 0.4854 0.1938 -0.0884 11.00000 0.05 0.44 Q28 1 0.1159 0.6766 0.2152 11.00000 0.05 0.43 Q29 1 0.2135 0.6313 0.4671 11.00000 0.05 0.43 Q30 1 0.2385 0.4978 0.4982 11.00000 0.05 0.43 Q31 1 0.6189 0.1156 0.5202 11.00000 0.05 0.43 Q32 1 0.7346 0.0679 0.3889 11.00000 0.05 0.41 Q33 1 0.2171 0.5242 0.4926 11.00000 0.05 0.41 Q34 1 0.6147 0.0927 0.1607 11.00000 0.05 0.40 Q35 1 0.2846 0.7084 0.1685 11.00000 0.05 0.40 Q36 1 0.6971 0.0467 0.4221 11.00000 0.05 0.39 Q37 1 0.7417 0.2052 0.4624 11.00000 0.05 0.38 Q38 1 0.1075 0.6666 0.2323 11.00000 0.05 0.38 Q39 1 0.0442 0.8036 0.2056 11.00000 0.05 0.38 Q40 1 0.2201 0.6348 0.2239 11.00000 0.05 0.37 ; _shelx_res_checksum 85634 _shelx_shelxl_version_number 2014/7 _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 3.213 _oxdiff_exptl_absorpt_empirical_full_min 0.485 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.18370(4) 0.62181(4) 0.26046(3) 0.02065(14) Uani 1 1 d . . . . . P2 P 0.28786(4) 0.64280(4) 0.16814(3) 0.02114(14) Uani 1 1 d . . . . . P3 P 0.05562(5) 0.73683(4) 0.19053(3) 0.02343(14) Uani 1 1 d . . . . . P4 P 0.15364(5) 0.51847(4) 0.21393(3) 0.02173(14) Uani 1 1 d . . . . . N1 N 0.32503(16) 0.79127(15) 0.20938(11) 0.0232(4) Uani 1 1 d . . . . . N2 N 0.24671(16) 0.83155(15) 0.10498(12) 0.0242(4) Uani 1 1 d . . . . . N3 N -0.09421(16) 0.70212(15) 0.29483(12) 0.0245(4) Uani 1 1 d . . . . . N4 N -0.09873(17) 0.67073(15) 0.19090(12) 0.0266(4) Uani 1 1 d . . . . . N5 N 0.33659(17) 0.36359(15) 0.27821(13) 0.0261(4) Uani 1 1 d . . . . . N6 N 0.32978(18) 0.41203(17) 0.15937(13) 0.0292(5) Uani 1 1 d . . . . . C1 C 0.28592(18) 0.75933(17) 0.16415(13) 0.0220(4) Uani 1 1 d . . . . . C2 C 0.3110(2) 0.88370(19) 0.17777(15) 0.0279(5) Uani 1 1 d . . . . . C3 C 0.2610(2) 0.90919(18) 0.11304(15) 0.0277(5) Uani 1 1 d . . . . . C4 C 0.3771(2) 0.73223(19) 0.28045(14) 0.0262(5) Uani 1 1 d . . . . . H4 H 0.3603 0.6760 0.2931 0.031 Uiso 1 1 calc R . . . . C5 C 0.3430(2) 0.7786(2) 0.34298(15) 0.0344(6) Uani 1 1 d . . . . . H5A H 0.3720 0.8250 0.3384 0.052 Uiso 1 1 calc GR . . . . H5B H 0.3646 0.7325 0.3883 0.052 Uiso 1 1 calc GR . . . . H5C H 0.2710 0.8075 0.3416 0.052 Uiso 1 1 calc GR . . . . C6 C 0.4906(2) 0.7009(2) 0.27214(16) 0.0312(6) Uani 1 1 d . . . . . H6A H 0.5096 0.6734 0.2318 0.047 Uiso 1 1 calc GR . . . . H6B H 0.5231 0.6558 0.3157 0.047 Uiso 1 1 calc GR . . . . H6C H 0.5105 0.7537 0.2636 0.047 Uiso 1 1 calc GR . . . . C7 C 0.2063(2) 0.8222(2) 0.03912(14) 0.0283(5) Uani 1 1 d . . . . . H7 H 0.1949 0.7632 0.0529 0.034 Uiso 1 1 calc R . . . . C8 C 0.2853(2) 0.8145(2) -0.01962(16) 0.0389(7) Uani 1 1 d . . . . . H8A H 0.2989 0.8711 -0.0342 0.058 Uiso 1 1 calc GR . . . . H8B H 0.2607 0.8047 -0.0608 0.058 Uiso 1 1 calc GR . . . . H8C H 0.3459 0.7630 -0.0009 0.058 Uiso 1 1 calc GR . . . . C9 C 0.1056(2) 0.8994(2) 0.01260(17) 0.0386(7) Uani 1 1 d . . . . . H9A H 0.0665 0.9152 0.0536 0.058 Uiso 1 1 calc GR . . . . H9B H 0.0701 0.8783 -0.0151 0.058 Uiso 1 1 calc GR . . . . H9C H 0.1168 0.9533 -0.0174 0.058 Uiso 1 1 calc GR . . . . C10 C 0.3485(3) 0.9411(2) 0.20960(17) 0.0366(6) Uani 1 1 d . . . . . H10A H 0.3058 0.9596 0.2484 0.055 Uiso 1 1 calc GR . . . . H10B H 0.3480 0.9956 0.1727 0.055 Uiso 1 1 calc GR . . . . H10C H 0.4158 0.9051 0.2282 0.055 Uiso 1 1 calc GR . . . . C11 C 0.2253(2) 1.0037(2) 0.06045(17) 0.0365(6) Uani 1 1 d . . . . . H11A H 0.2409 0.9974 0.0119 0.055 Uiso 1 1 calc GR . . . . H11B H 0.2582 1.0412 0.0715 0.055 Uiso 1 1 calc GR . . . . H11C H 0.1540 1.0332 0.0643 0.055 Uiso 1 1 calc GR . . . . C12 C 0.41577(19) 0.56759(17) 0.20035(13) 0.0226(5) Uani 1 1 d . . . . . C13 C 0.4432(2) 0.51099(18) 0.27062(14) 0.0247(5) Uani 1 1 d . . . . . H13 H 0.3951 0.5120 0.3064 0.030 Uiso 1 1 calc R . . . . C14 C 0.5433(2) 0.45282(19) 0.28692(15) 0.0289(5) Uani 1 1 d . . . . . H14 H 0.5615 0.4143 0.3335 0.035 Uiso 1 1 calc R . . . . C15 C 0.6157(2) 0.4519(2) 0.23461(16) 0.0321(6) Uani 1 1 d . . . . . H15 H 0.6824 0.4135 0.2463 0.039 Uiso 1 1 calc R . . . . C16 C 0.5891(2) 0.5081(2) 0.16448(15) 0.0309(5) Uani 1 1 d . . . . . H16 H 0.6380 0.5078 0.1293 0.037 Uiso 1 1 calc R . . . . C17 C 0.4898(2) 0.56447(19) 0.14716(14) 0.0266(5) Uani 1 1 d . . . . . H17 H 0.4718 0.6007 0.0999 0.032 Uiso 1 1 calc R . . . . C18 C -0.04942(18) 0.70171(17) 0.22970(14) 0.0230(5) Uani 1 1 d . . . . . C19 C -0.1737(2) 0.6726(2) 0.29658(16) 0.0306(6) Uani 1 1 d . . . . . C20 C -0.1757(2) 0.65206(19) 0.23215(16) 0.0311(6) Uani 1 1 d . . . . . C21 C -0.0660(2) 0.73753(19) 0.35127(15) 0.0279(5) Uani 1 1 d . . . . . H21 H 0.0010 0.7396 0.3390 0.033 Uiso 1 1 calc R . . . . C22 C -0.1356(3) 0.8369(2) 0.34738(18) 0.0387(6) Uani 1 1 d . . . . . H22A H -0.1406 0.8740 0.2982 0.058 Uiso 1 1 calc GR . . . . H22B H -0.1092 0.8620 0.3779 0.058 Uiso 1 1 calc GR . . . . H22C H -0.2010 0.8377 0.3636 0.058 Uiso 1 1 calc GR . . . . C23 C -0.0571(2) 0.6747(2) 0.42848(15) 0.0323(6) Uani 1 1 d . . . . . H23A H -0.1231 0.6808 0.4468 0.049 Uiso 1 1 calc GR . . . . H23B H -0.0225 0.6927 0.4592 0.049 Uiso 1 1 calc GR . . . . H23C H -0.0202 0.6110 0.4279 0.049 Uiso 1 1 calc GR . . . . C24 C -0.0806(2) 0.6717(2) 0.11252(15) 0.0329(6) Uani 1 1 d . . . . . H24 H -0.0154 0.6783 0.1011 0.039 Uiso 1 1 calc R . . . . C25 C -0.1590(3) 0.7577(3) 0.06544(18) 0.0479(8) Uani 1 1 d . . . . . H25A H -0.2247 0.7554 0.0766 0.072 Uiso 1 1 calc GR . . . . H25B H -0.1458 0.7593 0.0152 0.072 Uiso 1 1 calc GR . . . . H25C H -0.1560 0.8126 0.0749 0.072 Uiso 1 1 calc GR . . . . C26 C -0.0731(3) 0.5818(2) 0.0959(2) 0.0469(8) Uani 1 1 d . . . . . H26A H -0.0340 0.5295 0.1335 0.070 Uiso 1 1 calc GR . . . . H26B H -0.0412 0.5782 0.0501 0.070 Uiso 1 1 calc GR . . . . H26C H -0.1392 0.5807 0.0937 0.070 Uiso 1 1 calc GR . . . . C27 C -0.2441(2) 0.6682(3) 0.35826(18) 0.0428(7) Uani 1 1 d . . . . . H27A H -0.2123 0.6140 0.3969 0.064 Uiso 1 1 calc GR . . . . H27B H -0.3039 0.6648 0.3420 0.064 Uiso 1 1 calc GR . . . . H27C H -0.2615 0.7231 0.3756 0.064 Uiso 1 1 calc GR . . . . C28 C -0.2463(2) 0.6146(3) 0.2097(2) 0.0441(8) Uani 1 1 d . . . . . H28A H -0.2792 0.6548 0.1647 0.066 Uiso 1 1 calc GR . . . . H28B H -0.2956 0.6117 0.2465 0.066 Uiso 1 1 calc GR . . . . H28C H -0.2094 0.5533 0.2037 0.066 Uiso 1 1 calc GR . . . . C29 C 0.0372(2) 0.84125(19) 0.22057(17) 0.0302(5) Uani 1 1 d . . . . . C30 C 0.0925(2) 0.8444(2) 0.2750(2) 0.0384(7) Uani 1 1 d . . . . . H30 H 0.1406 0.7901 0.3018 0.046 Uiso 1 1 calc R . . . . C31 C 0.0756(3) 0.9300(3) 0.2893(3) 0.0551(10) Uani 1 1 d . . . . . H31 H 0.1126 0.9327 0.3258 0.066 Uiso 1 1 calc R . . . . C32 C 0.0043(3) 1.0108(2) 0.2495(3) 0.0585(11) Uani 1 1 d . . . . . H32 H -0.0065 1.0674 0.2593 0.070 Uiso 1 1 calc R . . . . C33 C -0.0510(3) 1.0078(2) 0.1952(2) 0.0488(8) Uani 1 1 d . . . . . H33 H -0.0993 1.0623 0.1688 0.059 Uiso 1 1 calc R . . . . C34 C -0.0345(2) 0.9237(2) 0.18006(19) 0.0378(6) Uani 1 1 d . . . . . H34 H -0.0711 0.9218 0.1429 0.045 Uiso 1 1 calc R . . . . C35 C 0.27922(19) 0.42715(18) 0.22079(14) 0.0245(5) Uani 1 1 d . . . . . C36 C 0.4236(2) 0.3078(2) 0.25217(18) 0.0330(6) Uani 1 1 d . . . . . C37 C 0.4191(2) 0.3387(2) 0.17817(17) 0.0346(6) Uani 1 1 d . . . . . C38 C 0.3039(2) 0.35345(18) 0.35574(14) 0.0270(5) Uani 1 1 d . . . . . H38 H 0.2485 0.4117 0.3574 0.032 Uiso 1 1 calc R . . . . C39 C 0.2610(2) 0.2760(2) 0.37807(19) 0.0376(6) Uani 1 1 d . . . . . H39A H 0.2045 0.2912 0.3471 0.056 Uiso 1 1 calc GR . . . . H39B H 0.2399 0.2698 0.4275 0.056 Uiso 1 1 calc GR . . . . H39C H 0.3118 0.2183 0.3736 0.056 Uiso 1 1 calc GR . . . . C40 C 0.3843(2) 0.33938(19) 0.40948(15) 0.0309(5) Uani 1 1 d . . . . . H40A H 0.4303 0.2758 0.4201 0.046 Uiso 1 1 calc GR . . . . H40B H 0.3532 0.3534 0.4535 0.046 Uiso 1 1 calc GR . . . . H40C H 0.4201 0.3801 0.3888 0.046 Uiso 1 1 calc GR . . . . C41 C 0.2858(2) 0.4643(2) 0.08395(15) 0.0328(6) Uani 1 1 d . . . . . H41 H 0.2310 0.5214 0.0887 0.039 Uiso 1 1 calc R . . . . C42 C 0.2383(3) 0.4088(3) 0.05560(19) 0.0426(7) Uani 1 1 d . . . . . H42A H 0.2886 0.3497 0.0536 0.064 Uiso 1 1 calc GR . . . . H42B H 0.2104 0.4428 0.0078 0.064 Uiso 1 1 calc GR . . . . H42C H 0.1860 0.3988 0.0875 0.064 Uiso 1 1 calc GR . . . . C43 C 0.3598(3) 0.4945(3) 0.03140(17) 0.0437(7) Uani 1 1 d . . . . . H43A H 0.4012 0.5128 0.0566 0.066 Uiso 1 1 calc GR . . . . H43B H 0.3234 0.5463 -0.0075 0.066 Uiso 1 1 calc GR . . . . H43C H 0.4014 0.4436 0.0120 0.066 Uiso 1 1 calc GR . . . . C44 C 0.5056(2) 0.2299(2) 0.2981(2) 0.0433(7) Uani 1 1 d . . . . . H44A H 0.5346 0.2536 0.3281 0.065 Uiso 1 1 calc GR . . . . H44B H 0.5564 0.1997 0.2677 0.065 Uiso 1 1 calc GR . . . . H44C H 0.4790 0.1858 0.3283 0.065 Uiso 1 1 calc GR . . . . C45 C 0.4963(3) 0.3025(3) 0.1249(2) 0.0484(8) Uani 1 1 d . . . . . H45A H 0.4645 0.2923 0.0875 0.073 Uiso 1 1 calc GR . . . . H45B H 0.5468 0.2449 0.1496 0.073 Uiso 1 1 calc GR . . . . H45C H 0.5270 0.3473 0.1037 0.073 Uiso 1 1 calc GR . . . . C46 C 0.08188(18) 0.46478(17) 0.28224(14) 0.0227(5) Uani 1 1 d . . . . . C47 C 0.05629(19) 0.48411(18) 0.34975(14) 0.0250(5) Uani 1 1 d . . . . . H47 H 0.0814 0.5226 0.3646 0.030 Uiso 1 1 calc R . . . . C48 C -0.0067(2) 0.44594(19) 0.39480(15) 0.0288(5) Uani 1 1 d . . . . . H48 H -0.0245 0.4600 0.4393 0.035 Uiso 1 1 calc R . . . . C49 C -0.0433(2) 0.3873(2) 0.37412(17) 0.0327(6) Uani 1 1 d . . . . . H49 H -0.0846 0.3612 0.4050 0.039 Uiso 1 1 calc R . . . . C50 C -0.0183(2) 0.3674(2) 0.30694(17) 0.0329(6) Uani 1 1 d . . . . . H50 H -0.0424 0.3277 0.2929 0.039 Uiso 1 1 calc R . . . . C51 C 0.0430(2) 0.40700(19) 0.26078(15) 0.0288(5) Uani 1 1 d . . . . . H51 H 0.0582 0.3950 0.2154 0.035 Uiso 1 1 calc R . . . . O5 O 0.76877(17) -0.12059(17) 0.18733(14) 0.0422(5) Uani 1 1 d . U . . . O6 O 0.6397(2) -0.0257(2) 0.09655(15) 0.0593(7) Uani 1 1 d . U . . . S2A S 0.6650(4) -0.0772(3) 0.1712(2) 0.0306(6) Uani 0.759(7) 1 d D U P A 1 F4A F 0.5246(3) 0.0646(4) 0.2080(3) 0.0568(14) Uani 0.759(7) 1 d D U P A 1 F5A F 0.6454(3) -0.0100(3) 0.28559(18) 0.0645(12) Uani 0.759(7) 1 d D U P A 1 F6A F 0.6708(3) 0.0766(2) 0.1892(2) 0.0573(10) Uani 0.759(7) 1 d D U P A 1 O4A O 0.6089(5) -0.1339(4) 0.2065(4) 0.0739(18) Uani 0.759(7) 1 d D U P A 1 C53A C 0.6225(3) 0.0163(4) 0.2162(3) 0.0400(11) Uani 0.759(7) 1 d D U P A 1 S2B S 0.6598(15) -0.0781(12) 0.1650(9) 0.037(2) Uani 0.241(7) 1 d D U P A 2 F4B F 0.5112(9) 0.0389(11) 0.2212(11) 0.058(4) Uani 0.241(7) 1 d D U P A 2 F5B F 0.6120(10) -0.0673(10) 0.2987(5) 0.082(5) Uani 0.241(7) 1 d D U P A 2 F6B F 0.6622(8) 0.0378(9) 0.2348(9) 0.069(3) Uani 0.241(7) 1 d D U P A 2 O4B O 0.6034(14) -0.1358(13) 0.1736(11) 0.056(3) Uani 0.241(7) 1 d D U P A 2 C53B C 0.6072(11) -0.0174(11) 0.2353(8) 0.051(3) Uani 0.241(7) 1 d D U P A 2 S3A S 0.95170(9) 0.29326(8) 0.07451(6) 0.0340(3) Uani 0.634(2) 1 d D U P B 1 F7A F 0.7786(3) 0.2906(4) 0.1321(3) 0.0554(11) Uani 0.634(2) 1 d D U P B 1 F8A F 0.8958(3) 0.2633(3) 0.20988(18) 0.0519(9) Uani 0.634(2) 1 d D U P B 1 F9A F 0.8184(4) 0.4028(4) 0.1442(3) 0.0491(12) Uani 0.634(2) 1 d D U P B 1 O7A O 1.0166(4) 0.3365(4) 0.0896(4) 0.0409(13) Uani 0.634(2) 1 d D U P B 1 O8A O 0.9965(4) 0.1945(3) 0.0879(3) 0.0442(10) Uani 0.634(2) 1 d D U P B 1 O9A O 0.8963(6) 0.3390(7) 0.0063(3) 0.0525(18) Uani 0.634(2) 1 d D U P B 1 C54A C 0.8592(3) 0.3100(3) 0.1441(2) 0.0187(7) Uani 0.634(2) 1 d D U P B 1 S1 S 0.24926(5) 0.57722(5) 0.46350(3) 0.02651(14) Uani 1 1 d . . . . . F1 F 0.38729(16) 0.59184(17) 0.53590(11) 0.0484(5) Uani 1 1 d . . . . . F2 F 0.28469(15) 0.53711(17) 0.60447(10) 0.0462(5) Uani 1 1 d . . . . . F3 F 0.39880(14) 0.45040(15) 0.54794(10) 0.0463(5) Uani 1 1 d . . . . . O1 O 0.18544(17) 0.66998(16) 0.46607(14) 0.0412(5) Uani 1 1 d . . . . . O2 O 0.19977(15) 0.51068(15) 0.47708(11) 0.0336(4) Uani 1 1 d . . . . . O3 O 0.31940(16) 0.57183(16) 0.40466(10) 0.0344(4) Uani 1 1 d . . . . . C52 C 0.3343(2) 0.5370(2) 0.54178(15) 0.0337(6) Uani 1 1 d . . . . . S3C S 0.8976(6) 0.3681(5) 0.0787(4) 0.0448(15) Uiso 0.115(2) 1 d D U P C 3 F7C F 0.8161(17) 0.2449(18) 0.1478(15) 0.059(4) Uiso 0.115(2) 1 d D U P C 3 F8C F 0.9725(18) 0.1877(11) 0.1170(13) 0.066(5) Uiso 0.115(2) 1 d D U P C 3 F9C F 0.933(2) 0.2505(16) 0.2068(9) 0.058(5) Uiso 0.115(2) 1 d D U P C 3 O8C O 0.880(3) 0.362(2) 0.0079(10) 0.054(5) Uiso 0.115(2) 1 d D U P C 3 O7C O 0.9995(13) 0.3631(17) 0.0884(16) 0.043(5) Uiso 0.115(2) 1 d D U P C 3 O9C O 0.8219(16) 0.4424(13) 0.1025(13) 0.052(4) Uiso 0.115(2) 1 d D U P C 3 C54C C 0.9011(15) 0.2608(11) 0.1390(10) 0.051(2) Uiso 0.115(2) 1 d D U P C 3 S3B S 0.8658(3) 0.3189(3) 0.1013(3) 0.0564(10) Uani 0.251(2) 1 d D U P D 2 F7B F 1.0051(9) 0.2368(7) 0.2029(5) 0.069(3) Uani 0.251(2) 1 d D U P D 2 F8B F 1.0381(9) 0.1806(7) 0.1077(7) 0.063(3) Uani 0.251(2) 1 d D U P D 2 F9B F 1.0482(8) 0.3138(9) 0.1035(7) 0.048(3) Uani 0.251(2) 1 d D U P D 2 O9B O 0.8346(13) 0.4051(10) 0.1207(9) 0.049(4) Uani 0.251(2) 1 d D U P D 2 O7B O 0.8751(14) 0.3312(14) 0.0226(6) 0.051(4) Uani 0.251(2) 1 d D U P D 2 O8B O 0.8157(12) 0.2555(12) 0.1342(10) 0.060(4) Uani 0.251(2) 1 d D U P D 2 C54B C 0.9944(7) 0.2602(8) 0.1302(6) 0.049(2) Uani 0.251(2) 1 d D U P D 2 Cl11 Cl 0.7632(12) 0.0801(10) 0.3500(9) 0.118(5) Uiso 0.150(4) 1 d D U P E 2 Cl12 Cl 0.8489(19) 0.2019(16) 0.3762(13) 0.156(5) Uiso 0.150(4) 1 d D U P E 2 C59B C 0.741(2) 0.178(3) 0.380(4) 0.133(5) Uiso 0.150(4) 1 d D U P E 2 H59A H 0.7174 0.1680 0.4295 0.159 Uiso 0.150(4) 1 calc R . P E 2 H59B H 0.6885 0.2305 0.3498 0.159 Uiso 0.150(4) 1 calc R . P E 2 Cl3A Cl 0.27664(16) 0.19783(15) 0.20318(10) 0.0469(4) Uani 0.745(5) 1 d D U P F 1 Cl4A Cl 0.15279(14) 0.12167(12) 0.30690(10) 0.0716(6) Uani 0.745(5) 1 d D U P F 1 C56A C 0.1663(4) 0.1724(4) 0.2164(4) 0.0593(14) Uani 0.745(5) 1 d D U P F 1 H56A H 0.1086 0.2295 0.2000 0.071 Uiso 0.745(5) 1 calc R . P F 1 H56B H 0.1684 0.1304 0.1875 0.071 Uiso 0.745(5) 1 calc R . P F 1 Cl9 Cl 0.78682(16) 0.22914(12) 0.36277(12) 0.0910(6) Uani 0.850(4) 1 d D U P E 1 Cl10 Cl 0.6738(3) 0.1530(2) 0.47492(13) 0.1273(10) Uani 0.850(4) 1 d D U P E 1 C59A C 0.7761(7) 0.1872(5) 0.4548(4) 0.102(2) Uani 0.850(4) 1 d D U P E 1 H59C H 0.7694 0.2353 0.4788 0.122 Uiso 0.850(4) 1 calc R . P E 1 H59D H 0.8369 0.1344 0.4735 0.122 Uiso 0.850(4) 1 calc R . P E 1 Cl6B Cl -0.0401(16) -0.0417(12) 0.5493(10) 0.183(6) Uani 0.236(7) 1 d D U P G -2 Cl5B Cl 0.0427(18) 0.1034(14) 0.4929(10) 0.176(5) Uani 0.236(7) 1 d D U P G -2 C57B C -0.065(2) 0.0769(17) 0.509(3) 0.177(7) Uani 0.236(7) 1 d D U P G -2 H57A H -0.1017 0.0950 0.4636 0.212 Uiso 0.236(7) 1 calc R . P G -2 H57B H -0.1084 0.1131 0.5408 0.212 Uiso 0.236(7) 1 calc R . P G -2 Cl2 Cl 0.39638(6) 0.14042(6) 0.05150(4) 0.04431(19) Uani 1 1 d D . . . . Cl1 Cl 0.47735(6) 0.23523(6) -0.07461(5) 0.0471(2) Uani 1 1 d D . . . . C55 C 0.4779(2) 0.1260(2) -0.02158(18) 0.0387(6) Uani 1 1 d D . . . . H55A H 0.4569 0.0956 -0.0514 0.046 Uiso 1 1 calc R . . . . H55B H 0.5455 0.0867 -0.0033 0.046 Uiso 1 1 calc R . . . . Cl8A Cl 0.4719(8) 0.1199(8) 0.5999(6) 0.117(3) Uani 0.204(3) 1 d D U P H -1 Cl7A Cl 0.4675(15) 0.0496(10) 0.4793(8) 0.187(6) Uani 0.204(3) 1 d D U P H -1 C58A C 0.501(3) 0.0257(15) 0.5672(12) 0.108(6) Uani 0.204(3) 1 d D U P H -1 H58A H 0.4681 -0.0148 0.5965 0.129 Uiso 0.204(3) 1 calc R . P H -1 H58B H 0.5728 -0.0084 0.5727 0.129 Uiso 0.204(3) 1 calc R . P H -1 Cl5A Cl 0.0989(18) 0.1099(13) 0.4727(11) 0.195(6) Uani 0.264(7) 1 d D U P G -1 Cl6A Cl -0.0253(17) -0.0005(16) 0.5062(12) 0.143(5) Uani 0.264(7) 1 d D U P G -1 C57A C 0.047(4) 0.047(3) 0.5401(13) 0.159(6) Uani 0.264(7) 1 d D U P G -1 H57C H 0.0051 0.0877 0.5693 0.191 Uiso 0.264(7) 1 calc R . P G -1 H57D H 0.1003 -0.0025 0.5713 0.191 Uiso 0.264(7) 1 calc R . P G -1 Cl4B Cl 0.2619(11) 0.1926(10) 0.2210(8) 0.125(4) Uani 0.255(5) 1 d D U P F 2 Cl3B Cl 0.2747(14) 0.0509(8) 0.3556(7) 0.185(5) Uani 0.255(5) 1 d D U P F 2 C56B C 0.2019(16) 0.1380(15) 0.2866(12) 0.096(4) Uani 0.255(5) 1 d D U P F 2 H56C H 0.1652 0.1121 0.2637 0.115 Uiso 0.255(5) 1 calc R . P F 2 H56D H 0.1528 0.1846 0.3078 0.115 Uiso 0.255(5) 1 calc R . P F 2 Cl7B Cl 0.5868(2) -0.0012(2) 0.62790(19) 0.0545(9) Uani 0.296(3) 1 d D U P H 3 Cl8B Cl 0.4012(3) 0.1017(3) 0.54425(19) 0.0654(10) Uani 0.296(3) 1 d D U P H 3 C58B C 0.5293(12) 0.049(2) 0.5420(9) 0.115(5) Uani 0.296(3) 1 d D U P H 3 H58C H 0.5570 0.0944 0.5149 0.138 Uiso 0.296(3) 1 calc R . P H 3 H58D H 0.5450 0.0005 0.5164 0.138 Uiso 0.296(3) 1 calc R . P H 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0208(3) 0.0240(3) 0.0189(3) -0.0021(2) -0.0026(2) -0.0118(2) P2 0.0206(3) 0.0265(3) 0.0180(3) -0.0015(2) -0.0033(2) -0.0127(2) P3 0.0210(3) 0.0249(3) 0.0232(3) 0.0007(2) -0.0028(2) -0.0113(2) P4 0.0239(3) 0.0256(3) 0.0186(3) -0.0035(2) -0.0002(2) -0.0137(2) N1 0.0247(10) 0.0267(10) 0.0203(10) -0.0010(8) -0.0024(8) -0.0147(8) N2 0.0207(9) 0.0284(10) 0.0210(10) -0.0001(8) -0.0024(8) -0.0101(8) N3 0.0187(9) 0.0274(10) 0.0237(10) 0.0025(8) -0.0049(8) -0.0097(8) N4 0.0246(10) 0.0275(10) 0.0271(11) 0.0005(8) -0.0098(8) -0.0120(8) N5 0.0243(10) 0.0262(10) 0.0303(11) -0.0099(9) 0.0023(8) -0.0107(8) N6 0.0299(11) 0.0398(12) 0.0259(11) -0.0133(9) 0.0046(9) -0.0191(10) C1 0.0209(11) 0.0272(11) 0.0186(10) 0.0000(9) -0.0029(8) -0.0131(9) C2 0.0299(13) 0.0266(12) 0.0286(13) -0.0038(10) 0.0002(10) -0.0141(10) C3 0.0269(12) 0.0258(12) 0.0282(13) -0.0009(10) 0.0006(10) -0.0113(10) C4 0.0294(13) 0.0319(13) 0.0210(11) -0.0009(10) -0.0066(9) -0.0179(10) C5 0.0431(16) 0.0427(15) 0.0247(13) -0.0060(11) -0.0061(11) -0.0245(13) C6 0.0283(13) 0.0346(14) 0.0328(13) -0.0008(11) -0.0088(10) -0.0173(11) C7 0.0272(12) 0.0353(13) 0.0191(11) 0.0014(10) -0.0070(9) -0.0120(11) C8 0.0369(15) 0.0517(18) 0.0250(13) -0.0059(12) -0.0021(11) -0.0150(13) C9 0.0288(14) 0.0461(17) 0.0293(14) 0.0036(12) -0.0122(11) -0.0074(12) C10 0.0469(17) 0.0303(14) 0.0379(15) -0.0041(12) -0.0045(13) -0.0220(13) C11 0.0410(16) 0.0283(13) 0.0338(14) 0.0034(11) -0.0027(12) -0.0128(12) C12 0.0231(11) 0.0265(11) 0.0210(11) -0.0026(9) -0.0034(9) -0.0137(9) C13 0.0269(12) 0.0287(12) 0.0207(11) -0.0024(9) -0.0031(9) -0.0147(10) C14 0.0303(13) 0.0299(13) 0.0258(12) 0.0010(10) -0.0097(10) -0.0137(11) C15 0.0230(12) 0.0358(14) 0.0353(14) -0.0048(11) -0.0089(10) -0.0094(10) C16 0.0246(12) 0.0418(15) 0.0283(13) -0.0092(11) 0.0004(10) -0.0142(11) C17 0.0248(12) 0.0345(13) 0.0210(11) -0.0025(10) -0.0026(9) -0.0139(10) C18 0.0194(11) 0.0235(11) 0.0240(11) 0.0008(9) -0.0058(9) -0.0092(9) C19 0.0201(11) 0.0336(13) 0.0325(13) 0.0062(11) -0.0079(10) -0.0123(10) C20 0.0227(12) 0.0313(13) 0.0366(14) 0.0040(11) -0.0092(10) -0.0138(10) C21 0.0242(12) 0.0306(13) 0.0258(12) -0.0033(10) -0.0048(9) -0.0083(10) C22 0.0387(16) 0.0323(14) 0.0370(15) -0.0051(12) -0.0029(12) -0.0057(12) C23 0.0311(13) 0.0355(14) 0.0232(12) -0.0032(11) -0.0019(10) -0.0066(11) C24 0.0352(14) 0.0355(14) 0.0273(13) -0.0047(11) -0.0118(11) -0.0121(11) C25 0.0500(19) 0.0469(18) 0.0300(15) 0.0017(13) -0.0131(14) -0.0043(15) C26 0.059(2) 0.0424(17) 0.0429(17) -0.0111(14) -0.0220(15) -0.0179(15) C27 0.0257(13) 0.0564(19) 0.0396(16) 0.0062(14) -0.0009(12) -0.0200(13) C28 0.0314(15) 0.0484(18) 0.057(2) -0.0036(15) -0.0149(14) -0.0240(14) C29 0.0254(12) 0.0259(12) 0.0395(15) -0.0029(11) 0.0005(11) -0.0134(10) C30 0.0318(14) 0.0302(14) 0.0562(19) -0.0105(13) -0.0060(13) -0.0139(11) C31 0.0464(19) 0.0405(18) 0.089(3) -0.0265(19) -0.0116(19) -0.0180(15) C32 0.054(2) 0.0304(16) 0.097(3) -0.0210(18) -0.004(2) -0.0174(15) C33 0.0426(18) 0.0271(14) 0.068(2) -0.0020(15) 0.0004(16) -0.0099(13) C34 0.0344(15) 0.0289(14) 0.0440(16) 0.0021(12) -0.0017(12) -0.0121(12) C35 0.0241(11) 0.0271(12) 0.0258(12) -0.0081(10) 0.0021(9) -0.0129(10) C36 0.0232(12) 0.0354(14) 0.0449(16) -0.0202(12) 0.0015(11) -0.0088(11) C37 0.0273(13) 0.0456(16) 0.0400(15) -0.0234(13) 0.0062(11) -0.0161(12) C38 0.0258(12) 0.0255(12) 0.0259(12) -0.0016(9) 0.0004(9) -0.0086(10) C39 0.0329(14) 0.0298(13) 0.0438(16) 0.0030(12) -0.0019(12) -0.0125(11) C40 0.0328(14) 0.0289(13) 0.0258(12) 0.0004(10) -0.0025(10) -0.0098(11) C41 0.0365(14) 0.0488(16) 0.0228(12) -0.0141(12) 0.0049(11) -0.0238(13) C42 0.0481(18) 0.0568(19) 0.0372(16) -0.0191(14) -0.0008(13) -0.0300(16) C43 0.0481(18) 0.068(2) 0.0289(14) -0.0185(14) 0.0089(13) -0.0344(17) C44 0.0307(15) 0.0412(16) 0.0541(19) -0.0217(15) -0.0039(13) -0.0013(13) C45 0.0346(16) 0.068(2) 0.0509(19) -0.0355(18) 0.0107(14) -0.0157(15) C46 0.0205(11) 0.0233(11) 0.0239(11) -0.0017(9) -0.0007(9) -0.0103(9) C47 0.0256(12) 0.0258(12) 0.0223(11) -0.0022(9) -0.0012(9) -0.0102(10) C48 0.0274(12) 0.0287(12) 0.0253(12) -0.0008(10) 0.0027(10) -0.0093(10) C49 0.0263(13) 0.0301(13) 0.0374(15) 0.0014(11) 0.0032(11) -0.0132(11) C50 0.0302(13) 0.0315(13) 0.0415(15) -0.0049(11) -0.0007(11) -0.0192(11) C51 0.0293(13) 0.0307(13) 0.0304(13) -0.0078(10) 0.0003(10) -0.0154(11) O5 0.0317(11) 0.0426(12) 0.0455(12) -0.0106(10) -0.0103(9) -0.0042(9) O6 0.0582(16) 0.0573(15) 0.0392(13) -0.0046(11) -0.0154(12) 0.0028(13) S2A 0.0276(10) 0.0304(8) 0.0328(9) 0.0014(7) -0.0089(8) -0.0142(7) F4A 0.0303(17) 0.068(3) 0.057(2) -0.024(2) -0.0104(15) 0.0066(17) F5A 0.0517(18) 0.085(3) 0.0321(16) -0.0163(17) -0.0127(13) 0.0058(17) F6A 0.0605(19) 0.0478(17) 0.071(2) -0.0256(17) 0.0043(16) -0.0214(14) O4A 0.055(3) 0.057(2) 0.110(5) 0.006(3) -0.004(3) -0.038(2) C53A 0.0292(19) 0.054(3) 0.031(2) -0.0093(18) -0.0092(16) -0.0072(19) S2B 0.028(3) 0.038(3) 0.045(3) -0.008(2) -0.011(2) -0.011(2) F4B 0.037(6) 0.056(7) 0.077(8) -0.024(6) -0.015(5) -0.003(5) F5B 0.068(7) 0.096(8) 0.032(4) -0.011(5) -0.002(4) 0.024(6) F6B 0.051(5) 0.068(6) 0.087(7) -0.038(6) -0.008(6) -0.007(5) O4B 0.043(6) 0.069(6) 0.083(8) -0.035(7) 0.005(6) -0.039(5) C53B 0.037(4) 0.054(5) 0.051(5) -0.011(4) -0.014(4) -0.002(4) S3A 0.0307(5) 0.0330(6) 0.0366(6) -0.0068(4) -0.0006(4) -0.0113(4) F7A 0.041(2) 0.077(3) 0.065(2) -0.028(2) 0.0064(19) -0.036(2) F8A 0.061(2) 0.066(2) 0.0333(16) -0.0117(14) 0.0002(15) -0.029(2) F9A 0.035(2) 0.048(2) 0.065(3) -0.030(2) 0.011(2) -0.0072(15) O7A 0.025(2) 0.037(3) 0.059(3) -0.006(3) -0.006(2) -0.012(2) O8A 0.045(3) 0.031(2) 0.052(3) -0.0167(18) 0.001(2) -0.0034(18) O9A 0.055(4) 0.063(4) 0.029(2) -0.003(2) 0.000(2) -0.016(3) C54A 0.0200(16) 0.0315(17) 0.0142(16) -0.0125(14) 0.0085(13) -0.0170(13) S1 0.0231(3) 0.0353(3) 0.0202(3) -0.0025(2) -0.0037(2) -0.0120(2) F1 0.0460(11) 0.0785(14) 0.0353(9) -0.0103(9) -0.0047(8) -0.0408(11) F2 0.0437(10) 0.0791(14) 0.0215(8) -0.0118(8) 0.0036(7) -0.0303(10) F3 0.0312(9) 0.0582(12) 0.0344(9) 0.0014(8) -0.0100(7) -0.0065(8) O1 0.0322(11) 0.0405(12) 0.0479(13) -0.0089(10) -0.0030(9) -0.0109(9) O2 0.0286(9) 0.0413(11) 0.0327(10) -0.0040(8) -0.0041(8) -0.0176(8) O3 0.0338(10) 0.0489(12) 0.0206(9) -0.0042(8) 0.0011(7) -0.0184(9) C52 0.0289(13) 0.0519(17) 0.0226(12) -0.0059(11) -0.0005(10) -0.0200(12) S3B 0.0401(17) 0.0494(18) 0.076(3) -0.0159(18) 0.0065(18) -0.0129(14) F7B 0.075(6) 0.066(5) 0.054(5) -0.010(4) 0.009(4) -0.018(5) F8B 0.060(6) 0.051(5) 0.067(6) -0.017(5) 0.003(5) -0.007(5) F9B 0.037(6) 0.047(6) 0.052(6) -0.007(4) 0.001(5) -0.013(5) O9B 0.043(6) 0.043(5) 0.054(7) -0.016(5) 0.021(5) -0.008(5) O7B 0.049(7) 0.057(6) 0.037(7) -0.003(5) -0.008(5) -0.013(5) O8B 0.049(6) 0.056(6) 0.070(7) -0.001(6) 0.004(6) -0.025(5) C54B 0.040(3) 0.042(3) 0.043(3) 0.000(3) 0.010(3) 0.001(3) Cl3A 0.0482(8) 0.0448(7) 0.0494(7) -0.0123(5) 0.0058(6) -0.0196(6) Cl4A 0.0823(11) 0.0743(10) 0.0920(12) -0.0438(9) 0.0363(9) -0.0578(9) C56A 0.046(3) 0.052(3) 0.089(4) -0.036(3) -0.008(3) -0.015(2) Cl9 0.0857(12) 0.0667(9) 0.1058(13) 0.0099(8) -0.0180(10) -0.0297(8) Cl10 0.191(3) 0.1316(19) 0.0781(13) -0.0109(12) 0.0056(15) -0.091(2) C59A 0.140(6) 0.070(4) 0.093(4) -0.015(3) -0.017(4) -0.037(4) Cl6B 0.260(14) 0.168(10) 0.142(10) -0.023(9) -0.020(10) -0.108(10) Cl5B 0.244(15) 0.190(9) 0.155(11) -0.071(8) 0.014(10) -0.133(10) C57B 0.263(15) 0.156(10) 0.139(11) -0.037(10) -0.002(11) -0.108(11) Cl2 0.0412(4) 0.0507(4) 0.0382(4) 0.0005(3) -0.0028(3) -0.0213(3) Cl1 0.0407(4) 0.0437(4) 0.0489(4) 0.0128(3) -0.0101(3) -0.0214(3) C55 0.0376(15) 0.0347(14) 0.0397(16) 0.0008(12) -0.0067(12) -0.0144(12) Cl8A 0.107(6) 0.142(6) 0.115(6) -0.030(5) 0.016(5) -0.066(5) Cl7A 0.187(10) 0.137(8) 0.154(9) 0.009(8) 0.002(8) 0.002(8) C58A 0.108(8) 0.091(8) 0.105(8) -0.009(8) 0.010(8) -0.028(8) Cl5A 0.300(17) 0.170(8) 0.172(11) -0.046(8) 0.012(11) -0.148(10) Cl6A 0.254(15) 0.100(4) 0.094(7) -0.007(4) -0.022(10) -0.096(10) C57A 0.257(15) 0.141(10) 0.134(11) -0.041(9) -0.002(11) -0.129(11) Cl4B 0.114(7) 0.111(6) 0.160(9) -0.065(6) 0.026(6) -0.038(5) Cl3B 0.238(11) 0.137(7) 0.169(9) -0.069(7) 0.017(8) -0.037(8) C56B 0.089(7) 0.082(7) 0.122(8) -0.038(7) 0.019(7) -0.034(7) Cl7B 0.0498(16) 0.0529(17) 0.0563(18) -0.0091(13) -0.0061(13) -0.0158(13) Cl8B 0.066(2) 0.080(2) 0.0462(17) -0.0024(15) -0.0125(14) -0.0285(18) C58B 0.117(8) 0.090(8) 0.113(8) -0.014(7) -0.001(8) -0.020(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 0 1 0.0545 0 0 -1 0.0545 0 1 0 0.1657 0 -1 0 0.1297 -8 0 -3 0.2153 -9 -4 -4 0.2539 9 5 1 0.2701 7 9 2 0.1528 0 -8 4 0.1161 -8 0 4 0.2039 6 8 9 0.1309 -7 -3 7 0.1929 6 2 10 0.1605 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 P1 P3 88.47(3) . . ? P2 P1 P4 89.35(3) . . ? P4 P1 P3 88.78(3) . . ? C1 P2 P1 101.91(8) . . ? C12 P2 P1 107.62(8) . . ? C12 P2 C1 102.66(11) . . ? C18 P3 P1 99.83(8) . . ? C29 P3 P1 105.33(10) . . ? C29 P3 C18 104.28(12) . . ? C35 P4 P1 101.20(8) . . ? C46 P4 P1 105.84(9) . . ? C46 P4 C35 103.90(11) . . ? C1 N1 C2 108.9(2) . . ? C1 N1 C4 123.9(2) . . ? C2 N1 C4 127.2(2) . . ? C1 N2 C3 109.2(2) . . ? C1 N2 C7 123.7(2) . . ? C3 N2 C7 126.8(2) . . ? C18 N3 C19 108.8(2) . . ? C18 N3 C21 124.1(2) . . ? C19 N3 C21 126.9(2) . . ? C18 N4 C20 108.7(2) . . ? C18 N4 C24 124.0(2) . . ? C20 N4 C24 126.6(2) . . ? C35 N5 C36 108.4(2) . . ? C35 N5 C38 124.0(2) . . ? C36 N5 C38 127.4(2) . . ? C35 N6 C37 108.9(2) . . ? C35 N6 C41 123.1(2) . . ? C37 N6 C41 127.7(2) . . ? N1 C1 P2 132.05(18) . . ? N2 C1 P2 120.56(18) . . ? N2 C1 N1 107.2(2) . . ? N1 C2 C10 124.5(2) . . ? C3 C2 N1 107.5(2) . . ? C3 C2 C10 128.1(3) . . ? N2 C3 C11 125.4(3) . . ? C2 C3 N2 107.2(2) . . ? C2 C3 C11 127.3(3) . . ? N1 C4 H4 107.1 . . ? N1 C4 C5 113.8(2) . . ? N1 C4 C6 110.2(2) . . ? C5 C4 H4 107.1 . . ? C6 C4 H4 107.1 . . ? C6 C4 C5 111.3(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7 107.1 . . ? N2 C7 C8 109.6(2) . . ? N2 C7 C9 112.7(2) . . ? C8 C7 H7 107.1 . . ? C9 C7 H7 107.1 . . ? C9 C7 C8 112.8(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 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P2 125.5(2) . . ? C13 C12 C17 119.2(2) . . ? C17 C12 P2 115.20(18) . . ? C12 C13 H13 120.2 . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13 120.2 . . ? C13 C14 H14 119.7 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.1(3) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 120.1 . . ? C17 C16 C15 119.8(3) . . ? C17 C16 H16 120.1 . . ? C12 C17 H17 119.7 . . ? C16 C17 C12 120.6(2) . . ? C16 C17 H17 119.7 . . ? N3 C18 P3 131.53(19) . . ? N3 C18 N4 107.7(2) . . ? N4 C18 P3 120.8(2) . . ? N3 C19 C27 124.5(3) . . ? C20 C19 N3 107.3(2) . . ? C20 C19 C27 128.2(3) . . ? N4 C20 C28 125.5(3) . . ? C19 C20 N4 107.5(2) . . ? C19 C20 C28 126.9(3) . . ? N3 C21 H21 106.4 . . ? N3 C21 C22 110.9(2) . . ? N3 C21 C23 114.4(2) . . ? C22 C21 H21 106.4 . . ? C22 C21 C23 111.6(2) . . ? C23 C21 H21 106.4 . . ? 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 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24 106.8 . . ? N4 C24 C25 109.6(3) . . ? N4 C24 C26 113.4(3) . . ? C25 C24 H24 106.8 . . ? C26 C24 H24 106.8 . . ? C26 C24 C25 113.1(3) . . ? 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 . . ? C19 C27 H27A 109.5 . . ? C19 C27 H27B 109.5 . . ? C19 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C20 C28 H28A 109.5 . . ? C20 C28 H28B 109.5 . . ? C20 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 P3 125.0(2) . . ? C30 C29 C34 119.8(3) . . ? C34 C29 P3 115.0(2) . . ? C29 C30 H30 120.3 . . ? C29 C30 C31 119.4(3) . . ? C31 C30 H30 120.3 . . ? C30 C31 H31 119.8 . . ? C32 C31 C30 120.4(4) . . ? C32 C31 H31 119.8 . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 120.0 . . ? C32 C33 C34 119.9(3) . . ? C34 C33 H33 120.0 . . ? C29 C34 H34 119.9 . . ? C33 C34 C29 120.2(3) . . ? C33 C34 H34 119.9 . . ? N5 C35 P4 132.6(2) . . ? N5 C35 N6 107.7(2) . . ? N6 C35 P4 119.7(2) . . ? N5 C36 C44 124.9(3) . . ? C37 C36 N5 107.5(3) . . ? C37 C36 C44 127.7(3) . . ? N6 C37 C45 124.4(3) . . ? C36 C37 N6 107.5(2) . . ? C36 C37 C45 128.0(3) . . ? N5 C38 H38 106.9 . . ? N5 C38 C39 109.6(2) . . ? N5 C38 C40 114.7(2) . . ? C39 C38 H38 106.9 . . ? C40 C38 H38 106.9 . . ? C40 C38 C39 111.5(2) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 H41 106.6 . . ? N6 C41 C42 110.3(3) . . ? N6 C41 C43 113.4(2) . . ? C42 C41 H41 106.6 . . ? C42 C41 C43 112.9(2) . . ? C43 C41 H41 106.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C36 C44 H44A 109.5 . . ? C36 C44 H44B 109.5 . . ? C36 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C37 C45 H45A 109.5 . . ? C37 C45 H45B 109.5 . . ? C37 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 P4 124.89(19) . . ? C47 C46 C51 119.1(2) . . ? C51 C46 P4 115.7(2) . . ? C46 C47 H47 120.0 . . ? C48 C47 C46 120.1(2) . . ? C48 C47 H47 120.0 . . ? C47 C48 H48 119.7 . . ? C49 C48 C47 120.7(3) . . ? C49 C48 H48 119.7 . . ? C48 C49 H49 120.1 . . ? C48 C49 C50 119.8(3) . . ? C50 C49 H49 120.1 . . ? C49 C50 H50 120.1 . . ? C51 C50 C49 119.9(3) . . ? C51 C50 H50 120.1 . . ? C46 C51 H51 119.8 . . ? C50 C51 C46 120.4(3) . . ? C50 C51 H51 119.8 . . ? O5 S2A O6 114.7(3) . . ? O5 S2A O4A 113.2(4) . . ? O5 S2A C53A 104.5(3) . . ? O6 S2A C53A 101.1(3) . . ? O4A S2A O6 118.2(5) . . ? O4A S2A C53A 102.4(4) . . ? F4A C53A S2A 113.2(4) . . ? F4A C53A F6A 107.7(5) . . ? F5A C53A S2A 114.6(4) . . ? F5A C53A F4A 108.3(4) . . ? F5A C53A F6A 102.6(5) . . ? F6A C53A S2A 109.8(3) . . ? O5 S2B C53B 100.5(9) . . ? O6 S2B O5 115.3(11) . . ? O6 S2B O4B 104.3(15) . . ? O6 S2B C53B 115.7(12) . . ? O4B S2B O5 119.6(15) . . ? O4B S2B C53B 101.0(10) . . ? F4B C53B S2B 112.3(11) . . ? F4B C53B F6B 107.5(13) . . ? F5B C53B S2B 116.5(12) . . ? F5B C53B F4B 107.2(13) . . ? F5B C53B F6B 106.9(13) . . ? F6B C53B S2B 106.0(11) . . ? O7A S3A O9A 114.6(5) . . ? O7A S3A C54A 102.9(3) . . ? O8A S3A O7A 114.4(3) . . ? O8A S3A O9A 114.0(4) . . ? O8A S3A C54A 103.5(3) . . ? O9A S3A C54A 105.7(3) . . ? F7A C54A S3A 113.0(3) . . ? F7A C54A F9A 103.5(4) . . ? F8A C54A S3A 113.5(3) . . ? F8A C54A F7A 109.4(4) . . ? F8A C54A F9A 106.6(4) . . ? F9A C54A S3A 110.1(3) . . ? O1 S1 O2 115.10(14) . . ? O1 S1 O3 115.13(14) . . ? O1 S1 C52 103.67(15) . . ? O2 S1 C52 104.04(13) . . ? O3 S1 O2 115.12(13) . . ? O3 S1 C52 101.19(13) . . ? F1 C52 S1 110.8(2) . . ? F1 C52 F2 107.6(2) . . ? F2 C52 S1 112.1(2) . . ? F3 C52 S1 111.5(2) . . ? F3 C52 F1 107.9(2) . . ? F3 C52 F2 106.8(3) . . ? O8C S3C O7C 112.4(14) . . ? O8C S3C O9C 115.0(13) . . ? O8C S3C C54C 105.6(11) . . ? O7C S3C C54C 100.7(10) . . ? O9C S3C O7C 113.4(12) . . ? O9C S3C C54C 108.3(10) . . ? F7C C54C S3C 117.1(13) . . ? F7C C54C F8C 107.8(14) . . ? F7C C54C F9C 105.8(14) . . ? F8C C54C S3C 109.7(12) . . ? F9C C54C S3C 111.8(12) . . ? F9C C54C F8C 103.6(14) . . ? O9B S3B O7B 112.3(10) . . ? O9B S3B O8B 117.9(9) . . ? O9B S3B C54B 105.1(8) . . ? O7B S3B C54B 100.8(8) . . ? O8B S3B O7B 112.4(10) . . ? O8B S3B C54B 106.3(8) . . ? F7B C54B S3B 112.0(8) . . ? F7B C54B F8B 107.5(10) . . ? F8B C54B S3B 111.8(9) . . ? F9B C54B S3B 111.4(8) . . ? F9B C54B F7B 106.7(11) . . ? F9B C54B F8B 107.1(10) . . ? Cl11 C59B Cl12 110.1(13) . . ? Cl11 C59B H59A 109.6 . . ? Cl11 C59B H59B 109.6 . . ? Cl12 C59B H59A 109.6 . . ? Cl12 C59B H59B 109.6 . . ? H59A C59B H59B 108.2 . . ? Cl3A C56A H56A 109.4 . . ? Cl3A C56A H56B 109.4 . . ? Cl4A C56A Cl3A 111.3(3) . . ? Cl4A C56A H56A 109.4 . . ? Cl4A C56A H56B 109.4 . . ? H56A C56A H56B 108.0 . . ? Cl9 C59A Cl10 112.2(5) . . ? Cl9 C59A H59C 109.2 . . ? Cl9 C59A H59D 109.2 . . ? Cl10 C59A H59C 109.2 . . ? Cl10 C59A H59D 109.2 . . ? H59C C59A H59D 107.9 . . ? Cl6B C57B H57A 109.0 . . ? Cl6B C57B H57B 109.0 . . ? Cl5B C57B Cl6B 112.9(14) . . ? Cl5B C57B H57A 109.0 . . ? Cl5B C57B H57B 109.0 . . ? H57A C57B H57B 107.8 . . ? Cl2 C55 Cl1 110.34(18) . . ? Cl2 C55 H55A 109.6 . . ? Cl2 C55 H55B 109.6 . . ? Cl1 C55 H55A 109.6 . . ? Cl1 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? Cl8A C58A Cl7A 114.8(13) . . ? Cl8A C58A H58A 108.6 . . ? Cl8A C58A H58B 108.6 . . ? Cl7A C58A H58A 108.6 . . ? Cl7A C58A H58B 108.6 . . ? H58A C58A H58B 107.6 . . ? Cl5A C57A Cl6A 112.5(13) . . ? Cl5A C57A H57C 109.1 . . ? Cl5A C57A H57D 109.1 . . ? Cl6A C57A H57C 109.1 . . ? Cl6A C57A H57D 109.1 . . ? H57C C57A H57D 107.8 . . ? Cl4B C56B Cl3B 117.0(13) . . ? Cl4B C56B H56C 108.0 . . ? Cl4B C56B H56D 108.0 . . ? Cl3B C56B H56C 108.0 . . ? Cl3B C56B H56D 108.0 . . ? H56C C56B H56D 107.3 . . ? Cl7B C58B H58C 108.9 . . ? Cl7B C58B H58D 108.9 . . ? Cl8B C58B Cl7B 113.5(10) . . ? Cl8B C58B H58C 108.9 . . ? Cl8B C58B H58D 108.9 . . ? H58C C58B H58D 107.7 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 P2 2.2545(8) . ? P1 P3 2.2596(8) . ? P1 P4 2.2582(8) . ? P2 C1 1.835(3) . ? P2 C12 1.825(3) . ? P3 C18 1.834(3) . ? P3 C29 1.832(3) . ? P4 C35 1.836(3) . ? P4 C46 1.827(3) . ? N1 C1 1.362(3) . ? N1 C2 1.382(3) . ? N1 C4 1.498(3) . ? N2 C1 1.359(3) . ? N2 C3 1.381(4) . ? N2 C7 1.494(3) . ? N3 C18 1.354(3) . ? N3 C19 1.382(3) . ? N3 C21 1.491(3) . ? N4 C18 1.357(3) . ? N4 C20 1.380(4) . ? N4 C24 1.497(4) . ? N5 C35 1.356(4) . ? N5 C36 1.382(3) . ? N5 C38 1.503(3) . ? N6 C35 1.359(3) . ? N6 C37 1.369(4) . ? N6 C41 1.511(4) . ? C2 C3 1.367(4) . ? C2 C10 1.493(4) . ? C3 C11 1.500(4) . ? C4 H4 0.9800 . ? C4 C5 1.527(4) . ? C4 C6 1.522(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7 0.9800 . ? C7 C8 1.524(4) . ? C7 C9 1.523(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.395(3) . ? C12 C17 1.405(4) . ? C13 H13 0.9300 . ? C13 C14 1.395(4) . ? C14 H14 0.9300 . ? C14 C15 1.380(4) . ? C15 H15 0.9300 . ? C15 C16 1.390(4) . ? C16 H16 0.9300 . ? C16 C17 1.382(4) . ? C17 H17 0.9300 . ? C19 C20 1.363(4) . ? C19 C27 1.493(4) . ? C20 C28 1.493(4) . ? C21 H21 0.9800 . ? C21 C22 1.515(4) . ? C21 C23 1.531(4) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24 0.9800 . ? C24 C25 1.521(4) . ? C24 C26 1.519(4) . ? 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 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.382(4) . ? C29 C34 1.402(4) . ? C30 H30 0.9300 . ? C30 C31 1.398(5) . ? C31 H31 0.9300 . ? C31 C32 1.381(6) . ? C32 H32 0.9300 . ? C32 C33 1.376(6) . ? C33 H33 0.9300 . ? C33 C34 1.384(5) . ? C34 H34 0.9300 . ? C36 C37 1.366(5) . ? C36 C44 1.482(4) . ? C37 C45 1.501(4) . ? C38 H38 0.9800 . ? C38 C39 1.528(4) . ? C38 C40 1.521(4) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41 0.9800 . ? C41 C42 1.521(4) . ? C41 C43 1.522(4) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.397(4) . ? C46 C51 1.400(4) . ? C47 H47 0.9300 . ? C47 C48 1.390(4) . ? C48 H48 0.9300 . ? C48 C49 1.384(4) . ? C49 H49 0.9300 . ? C49 C50 1.393(5) . ? C50 H50 0.9300 . ? C50 C51 1.393(4) . ? C51 H51 0.9300 . ? O5 S2A 1.408(6) . ? O5 S2B 1.50(2) . ? O6 S2A 1.441(5) . ? O6 S2B 1.339(19) . ? S2A O4A 1.431(5) . ? S2A C53A 1.812(6) . ? F4A C53A 1.325(5) . ? F5A C53A 1.309(6) . ? F6A C53A 1.360(7) . ? S2B O4B 1.409(15) . ? S2B C53B 1.818(14) . ? F4B C53B 1.337(14) . ? F5B C53B 1.251(15) . ? F6B C53B 1.384(16) . ? S3A O7A 1.435(6) . ? S3A O8A 1.424(5) . ? S3A O9A 1.445(7) . ? S3A C54A 1.800(4) . ? F7A C54A 1.355(5) . ? F8A C54A 1.313(6) . ? F9A C54A 1.379(6) . ? S1 O1 1.436(2) . ? S1 O2 1.445(2) . ? S1 O3 1.445(2) . ? S1 C52 1.827(3) . ? F1 C52 1.337(4) . ? F2 C52 1.343(3) . ? F3 C52 1.329(4) . ? S3C O8C 1.431(15) . ? S3C O7C 1.458(15) . ? S3C O9C 1.432(14) . ? S3C C54C 1.777(13) . ? F7C C54C 1.324(16) . ? F8C C54C 1.377(16) . ? F9C C54C 1.361(17) . ? S3B O9B 1.425(13) . ? S3B O7B 1.466(12) . ? S3B O8B 1.436(12) . ? S3B C54B 1.784(10) . ? F7B C54B 1.345(13) . ? F8B C54B 1.363(13) . ? F9B C54B 1.335(14) . ? Cl11 C59B 1.719(16) . ? Cl12 C59B 1.723(16) . ? C59B H59A 0.9700 . ? C59B H59B 0.9700 . ? Cl3A C56A 1.758(6) . ? Cl4A C56A 1.732(7) . ? C56A H56A 0.9700 . ? C56A H56B 0.9700 . ? Cl9 C59A 1.723(8) . ? Cl10 C59A 1.729(9) . ? C59A H59C 0.9700 . ? C59A H59D 0.9700 . ? Cl6B C57B 1.752(16) . ? Cl5B C57B 1.737(16) . ? C57B H57A 0.9700 . ? C57B H57B 0.9700 . ? Cl2 C55 1.754(4) . ? Cl1 C55 1.766(3) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? Cl8A C58A 1.684(16) . ? Cl7A C58A 1.688(15) . ? C58A H58A 0.9700 . ? C58A H58B 0.9700 . ? Cl5A C57A 1.709(16) . ? Cl6A C57A 1.747(16) . ? C57A H57C 0.9700 . ? C57A H57D 0.9700 . ? Cl4B C56B 1.695(15) . ? Cl3B C56B 1.710(15) . ? C56B H56C 0.9700 . ? C56B H56D 0.9700 . ? Cl7B C58B 1.743(15) . ? Cl8B C58B 1.714(15) . ? C58B H58C 0.9700 . ? C58B H58D 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 P2 C1 N1 71.0(2) . . . . ? P1 P2 C1 N2 -114.93(19) . . . . ? P1 P2 C12 C13 -2.7(2) . . . . ? P1 P2 C12 C17 173.54(17) . . . . ? P1 P3 C18 N3 70.1(2) . . . . ? P1 P3 C18 N4 -111.81(19) . . . . ? P1 P3 C29 C30 0.0(3) . . . . ? P1 P3 C29 C34 175.2(2) . . . . ? P1 P4 C35 N5 70.5(3) . . . . ? P1 P4 C35 N6 -112.48(19) . . . . ? P1 P4 C46 C47 -2.1(2) . . . . ? P1 P4 C46 C51 171.68(18) . . . . ? P2 C12 C13 C14 176.4(2) . . . . ? P2 C12 C17 C16 -178.3(2) . . . . ? P3 C29 C30 C31 175.5(3) . . . . ? P3 C29 C34 C33 -176.5(3) . . . . ? P4 C46 C47 C48 173.8(2) . . . . ? P4 C46 C51 C50 -175.9(2) . . . . ? N1 C2 C3 N2 -1.2(3) . . . . ? N1 C2 C3 C11 177.5(3) . . . . ? N3 C19 C20 N4 -1.1(3) . . . . ? N3 C19 C20 C28 177.9(3) . . . . ? N5 C36 C37 N6 -0.5(3) . . . . ? N5 C36 C37 C45 178.5(3) . . . . ? C1 P2 C12 C13 104.4(2) . . . . ? C1 P2 C12 C17 -79.4(2) . . . . ? C1 N1 C2 C3 1.1(3) . . . . ? C1 N1 C2 C10 -176.8(3) . . . . ? C1 N1 C4 C5 -133.7(3) . . . . ? C1 N1 C4 C6 100.5(3) . . . . ? C1 N2 C3 C2 0.8(3) . . . . ? C1 N2 C3 C11 -177.9(3) . . . . ? C1 N2 C7 C8 -99.0(3) . . . . ? C1 N2 C7 C9 134.4(3) . . . . ? C2 N1 C1 P2 174.1(2) . . . . ? C2 N1 C1 N2 -0.6(3) . . . . ? C2 N1 C4 C5 48.3(3) . . . . ? C2 N1 C4 C6 -77.5(3) . . . . ? C3 N2 C1 P2 -175.53(18) . . . . ? C3 N2 C1 N1 -0.1(3) . . . . ? C3 N2 C7 C8 73.2(3) . . . . ? C3 N2 C7 C9 -53.3(4) . . . . ? C4 N1 C1 P2 -4.2(4) . . . . ? C4 N1 C1 N2 -178.9(2) . . . . ? C4 N1 C2 C3 179.4(2) . . . . ? C4 N1 C2 C10 1.4(4) . . . . ? C7 N2 C1 P2 -2.1(3) . . . . ? C7 N2 C1 N1 173.3(2) . . . . ? C7 N2 C3 C2 -172.4(2) . . . . ? C7 N2 C3 C11 8.9(4) . . . . ? C10 C2 C3 N2 176.7(3) . . . . ? C10 C2 C3 C11 -4.7(5) . . . . ? C12 P2 C1 N1 -40.4(3) . . . . ? C12 P2 C1 N2 133.7(2) . . . . ? C12 C13 C14 C15 1.1(4) . . . . ? C13 C12 C17 C16 -1.8(4) . . . . ? C13 C14 C15 C16 -1.0(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C12 2.0(4) . . . . ? C17 C12 C13 C14 0.3(4) . . . . ? C18 P3 C29 C30 104.6(3) . . . . ? C18 P3 C29 C34 -80.2(2) . . . . ? C18 N3 C19 C20 1.3(3) . . . . ? C18 N3 C19 C27 -176.9(3) . . . . ? C18 N3 C21 C22 97.3(3) . . . . ? C18 N3 C21 C23 -135.3(3) . . . . ? C18 N4 C20 C19 0.5(3) . . . . ? C18 N4 C20 C28 -178.6(3) . . . . ? C18 N4 C24 C25 -97.3(3) . . . . ? C18 N4 C24 C26 135.3(3) . . . . ? C19 N3 C18 P3 177.2(2) . . . . ? C19 N3 C18 N4 -1.0(3) . . . . ? C19 N3 C21 C22 -76.7(3) . . . . ? C19 N3 C21 C23 50.7(3) . . . . ? C20 N4 C18 P3 -178.13(18) . . . . ? C20 N4 C18 N3 0.3(3) . . . . ? C20 N4 C24 C25 72.7(4) . . . . ? C20 N4 C24 C26 -54.7(4) . . . . ? C21 N3 C18 P3 2.3(4) . . . . ? C21 N3 C18 N4 -175.9(2) . . . . ? C21 N3 C19 C20 176.0(2) . . . . ? C21 N3 C19 C27 -2.3(4) . . . . ? C24 N4 C18 P3 -6.7(3) . . . . ? C24 N4 C18 N3 171.8(2) . . . . ? C24 N4 C20 C19 -170.7(2) . . . . ? C24 N4 C20 C28 10.2(4) . . . . ? C27 C19 C20 N4 177.1(3) . . . . ? C27 C19 C20 C28 -3.9(5) . . . . ? C29 P3 C18 N3 -38.6(3) . . . . ? C29 P3 C18 N4 139.5(2) . . . . ? C29 C30 C31 C32 0.0(6) . . . . ? C30 C29 C34 C33 -1.0(5) . . . . ? C30 C31 C32 C33 0.0(7) . . . . ? C31 C32 C33 C34 -0.5(7) . . . . ? C32 C33 C34 C29 1.0(6) . . . . ? C34 C29 C30 C31 0.5(5) . . . . ? C35 P4 C46 C47 104.0(2) . . . . ? C35 P4 C46 C51 -82.2(2) . . . . ? C35 N5 C36 C37 0.5(3) . . . . ? C35 N5 C36 C44 -179.9(3) . . . . ? C35 N5 C38 C39 96.3(3) . . . . ? C35 N5 C38 C40 -137.4(2) . . . . ? C35 N6 C37 C36 0.2(3) . . . . ? C35 N6 C37 C45 -178.8(3) . . . . ? C35 N6 C41 C42 -94.9(3) . . . . ? C35 N6 C41 C43 137.3(3) . . . . ? C36 N5 C35 P4 176.9(2) . . . . ? C36 N5 C35 N6 -0.4(3) . . . . ? C36 N5 C38 C39 -78.4(3) . . . . ? C36 N5 C38 C40 48.0(4) . . . . ? C37 N6 C35 P4 -177.59(19) . . . . ? C37 N6 C35 N5 0.1(3) . . . . ? C37 N6 C41 C42 78.8(4) . . . . ? C37 N6 C41 C43 -49.0(4) . . . . ? C38 N5 C35 P4 1.4(4) . . . . ? C38 N5 C35 N6 -175.9(2) . . . . ? C38 N5 C36 C37 175.9(2) . . . . ? C38 N5 C36 C44 -4.6(4) . . . . ? C41 N6 C35 P4 -2.9(3) . . . . ? C41 N6 C35 N5 174.8(2) . . . . ? C41 N6 C37 C36 -174.2(2) . . . . ? C41 N6 C37 C45 6.8(5) . . . . ? C44 C36 C37 N6 -180.0(3) . . . . ? C44 C36 C37 C45 -1.0(5) . . . . ? C46 P4 C35 N5 -39.1(3) . . . . ? C46 P4 C35 N6 137.9(2) . . . . ? C46 C47 C48 C49 1.2(4) . . . . ? C47 C46 C51 C50 -1.7(4) . . . . ? C47 C48 C49 C50 -1.1(4) . . . . ? C48 C49 C50 C51 -0.4(4) . . . . ? C49 C50 C51 C46 1.7(4) . . . . ? C51 C46 C47 C48 0.2(4) . . . . ? O5 S2A C53A F4A -178.9(4) . . . . ? O5 S2A C53A F5A -54.0(5) . . . . ? O5 S2A C53A F6A 60.8(4) . . . . ? O5 S2B C53B F4B 170.3(13) . . . . ? O5 S2B C53B F5B -65.6(15) . . . . ? O5 S2B C53B F6B 53.1(13) . . . . ? O6 S2A C53A F4A 61.8(6) . . . . ? O6 S2A C53A F5A -173.4(5) . . . . ? O6 S2A C53A F6A -58.6(4) . . . . ? O6 S2B C53B F4B 45.4(18) . . . . ? O6 S2B C53B F5B 169.5(15) . . . . ? O6 S2B C53B F6B -71.8(15) . . . . ? O4A S2A C53A F4A -60.6(6) . . . . ? O4A S2A C53A F5A 64.2(6) . . . . ? O4A S2A C53A F6A 179.0(4) . . . . ? O4B S2B C53B F4B -66.5(19) . . . . ? O4B S2B C53B F5B 57.6(19) . . . . ? O4B S2B C53B F6B 176.3(15) . . . . ? O7A S3A C54A F7A 167.8(4) . . . . ? O7A S3A C54A F8A -66.8(4) . . . . ? O7A S3A C54A F9A 52.6(4) . . . . ? O8A S3A C54A F7A -72.9(4) . . . . ? O8A S3A C54A F8A 52.5(4) . . . . ? O8A S3A C54A F9A 171.9(4) . . . . ? O9A S3A C54A F7A 47.3(6) . . . . ? O9A S3A C54A F8A 172.6(5) . . . . ? O9A S3A C54A F9A -67.9(5) . . . . ? O1 S1 C52 F1 -60.4(2) . . . . ? O1 S1 C52 F2 59.7(3) . . . . ? O1 S1 C52 F3 179.3(2) . . . . ? O2 S1 C52 F1 178.8(2) . . . . ? O2 S1 C52 F2 -61.0(3) . . . . ? O2 S1 C52 F3 58.6(2) . . . . ? O3 S1 C52 F1 59.1(2) . . . . ? O3 S1 C52 F2 179.3(2) . . . . ? O3 S1 C52 F3 -61.1(2) . . . . ? O8C S3C C54C F7C -68(2) . . . . ? O8C S3C C54C F8C 56(2) . . . . ? O8C S3C C54C F9C 170(2) . . . . ? O7C S3C C54C F7C 175(2) . . . . ? O7C S3C C54C F8C -61.5(18) . . . . ? O7C S3C C54C F9C 52.9(19) . . . . ? O9C S3C C54C F7C 56(2) . . . . ? O9C S3C C54C F8C 179.3(17) . . . . ? O9C S3C C54C F9C -66.3(19) . . . . ? O9B S3B C54B F7B 66.2(12) . . . . ? O9B S3B C54B F8B -173.0(10) . . . . ? O9B S3B C54B F9B -53.3(12) . . . . ? O7B S3B C54B F7B -177.0(12) . . . . ? O7B S3B C54B F8B -56.2(12) . . . . ? O7B S3B C54B F9B 63.6(13) . . . . ? O8B S3B C54B F7B -59.5(13) . . . . ? O8B S3B C54B F8B 61.3(13) . . . . ? O8B S3B C54B F9B -179.0(13) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0000 -0.0000 1.0000 -0.0835 -0.0013 0.0056 0.0000 0.0000 -1.0000 0.0835 0.0013 -0.0056 -0.0000 1.0000 0.0000 0.0207 0.0016 -0.1054 0.0000 -1.0000 -0.0000 -0.0207 -0.0016 0.1054 -8.0000 0.0000 -3.0001 0.2596 -0.8513 -0.3727 -9.0000 -4.0000 -4.0002 0.2613 -0.9632 -0.0014 9.0000 5.0000 1.0002 0.0098 0.9688 -0.1208 7.0000 9.0000 2.0002 0.0116 0.7600 -0.6256 0.0001 -8.0000 3.9999 -0.4997 -0.0181 0.8652 -8.0000 0.0000 3.9999 -0.3247 -0.8607 -0.3335 5.9999 8.0000 9.0002 -0.5923 0.6421 -0.5255 -7.0000 -3.0000 6.9998 -0.6384 -0.7626 0.0438 6.0000 2.0000 10.0001 -0.8001 0.6312 0.1122