#------------------------------------------------------------------------------ #$Date: 2023-11-15 01:36:00 +0200 (Wed, 15 Nov 2023) $ #$Revision: 287595 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247720.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_7247720 loop_ _publ_author_name 'Madhesiya, Avinash' 'Dash, Sibananda G.' 'Gupta, Princi' 'Akhir, Abdul' 'Saxena, Deepanshi' 'Maitra, Rahul' 'Chopra, Sidharth' 'Thakur, Tejender S.' _publ_section_title ; Development of New Multi-component Crystals of the Antifungal Drug Tioconazole and the Assessment of their Biopharmaceutical Attributes ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00948C _journal_year 2023 _chemical_formula_moiety '2(C16 H14 Cl3 N2 O S), O4 S, 7(H2 O)' _chemical_formula_sum 'C32 H42 Cl6 N4 O13 S3' _chemical_formula_weight 999.57 _chemical_name_common 'Tioconzaole sulfate (2:1) salt heptahydrate' _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2019/2 _audit_update_record ; 2023-09-22 deposited with the CCDC. 2023-11-14 downloaded from the CCDC. ; _cell_angle_alpha 86.078(2) _cell_angle_beta 77.368(2) _cell_angle_gamma 66.240(3) _cell_formula_units_Z 2 _cell_length_a 10.5568(3) _cell_length_b 10.9083(3) _cell_length_c 20.8988(4) _cell_measurement_reflns_used 18112 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 79.3000 _cell_measurement_theta_min 2.1740 _cell_volume 2148.81(11) _computing_cell_refinement 'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXL-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.962 _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 -24.00 24.00 0.50 0.09 -- -47.08 19.00 60.00 96 2 \w -62.00 24.00 0.50 0.09 -- -47.08 57.00 60.00 172 3 \w -17.00 25.00 0.50 0.09 -- -47.08 38.00 -60.00 84 4 \w -25.00 25.00 0.50 0.09 -- -47.08 38.00-180.00 100 5 \w 130.00 177.00 0.50 0.37 -- 113.25 77.00 -30.00 94 6 \w 140.00 177.00 0.50 0.37 -- 113.25 45.00 0.00 74 7 \w 96.00 121.00 0.50 0.37 -- 113.25 77.00 -30.00 50 8 \w 102.00 177.00 0.50 0.37 -- 113.25 61.00 -60.00 150 9 \w 98.00 152.00 0.50 0.37 -- 113.25 61.00-120.00 108 10 \w 102.00 138.00 0.50 0.37 -- 113.25 45.00-120.00 72 11 \w 103.00 169.00 0.50 0.37 -- 113.25 30.00 -60.00 132 12 \w 101.00 155.00 0.50 0.37 -- 113.25 30.00 30.00 108 13 \w 101.00 178.00 0.50 0.37 -- 113.25 30.00 60.00 154 14 \w 142.00 167.00 0.50 0.37 -- 113.25 30.00 90.00 50 15 \w 105.00 143.00 0.50 0.37 -- 113.25 30.00 120.00 76 16 \w 106.00 178.00 0.50 0.37 -- 113.25 30.00 150.00 144 17 \w 102.00 140.00 0.50 0.37 -- 113.25 30.00 90.00 76 18 \w 149.00 176.00 0.50 0.37 -- 113.25 94.00 -19.00 54 19 \w 43.00 69.00 0.50 0.37 -- 113.25 -61.00 120.00 52 20 \w 67.00 92.00 0.50 0.37 -- 113.25 -77.00 90.00 50 21 \w 43.00 70.00 0.50 0.37 -- 113.25 -61.00 90.00 54 22 \w 42.00 73.00 0.50 0.37 -- 113.25 -61.00 60.00 62 23 \w 47.00 73.00 0.50 0.37 -- 113.25 -61.00 -60.00 52 24 \w 42.00 68.00 0.50 0.37 -- 113.25 -61.00-120.00 52 25 \w 59.00 95.00 0.50 0.37 -- 113.25 -94.00-129.00 72 26 \w 78.00 109.00 0.50 0.37 -- 113.25-114.00-150.00 62 27 \w 45.00 71.00 0.50 0.37 -- 113.25-114.00-150.00 52 28 \w 75.00 106.00 0.50 0.37 -- 113.25 -99.00 -90.50 62 29 \w 79.00 104.00 0.50 0.37 -- 113.25 -95.00 -30.00 50 30 \w 54.00 93.00 0.50 0.37 -- 113.25 -95.00 -90.00 78 31 \w 43.00 93.00 0.50 0.37 -- 113.25 -95.00 60.00 100 32 \w 49.00 107.00 0.50 0.37 -- 113.25-104.00 123.35 116 33 \w 53.00 94.00 0.50 0.37 -- 113.25 -95.00 150.00 82 34 \w 73.00 123.00 0.50 0.37 -- 113.25-140.00 118.49 100 35 \w 57.00 96.00 0.50 0.37 -- 113.25 -95.00 0.00 78 36 \w 46.00 103.00 0.50 0.37 -- 113.25 -95.00 30.00 114 37 \w 46.00 72.00 0.50 0.37 -- 113.25 -95.00 -30.00 52 38 \w 44.00 104.00 0.50 0.37 -- 113.25 -95.00 -60.00 120 39 \w 59.00 106.00 0.50 0.37 -- 113.25 -95.00-150.00 94 40 \w 53.00 100.00 0.50 0.37 -- 113.25 -95.00-180.00 94 41 \w 35.00 89.00 0.50 0.09 -- 47.08-125.00-120.00 108 42 \w 40.00 78.00 0.50 0.09 -- 47.08 -94.00-129.00 76 43 \w -12.00 31.00 0.50 0.09 -- 47.08 -94.00-129.00 86 44 \w -45.00 -18.00 0.50 0.09 -- -47.08 94.00 -19.00 54 45 \w -13.00 12.00 0.50 0.09 -- -47.08 94.00 -19.00 50 46 \w -49.00 -21.00 0.50 0.37 -- -91.75 45.00 60.00 56 47 \w -74.00 -49.00 0.50 0.37 -- -91.75 94.00 -19.00 50 48 \w -49.00 -21.00 0.50 0.37 -- -91.75 45.00 0.00 56 49 \w -115.00 -34.00 0.50 0.09 -- -47.08 -57.00 -90.00 162 50 \w -163.00-107.00 0.50 0.37 -- -91.75 -95.00 -30.00 112 51 \w -123.00 -91.00 0.50 0.37 -- -91.75 -94.00-129.00 64 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0804003000 _diffrn_orient_matrix_UB_12 0.0778925000 _diffrn_orient_matrix_UB_13 0.0189489000 _diffrn_orient_matrix_UB_21 0.1018477000 _diffrn_orient_matrix_UB_22 -0.0354203000 _diffrn_orient_matrix_UB_23 -0.0675321000 _diffrn_orient_matrix_UB_31 -0.0987452000 _diffrn_orient_matrix_UB_32 0.1284549000 _diffrn_orient_matrix_UB_33 -0.0281073000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.0610 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.962 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 28515 _diffrn_reflns_point_group_measured_fraction_full 0.696 _diffrn_reflns_point_group_measured_fraction_max 0.657 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.287 _diffrn_reflns_theta_min 2.167 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.575 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.49291 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.545 _exptl_crystal_description plate _exptl_crystal_F_000 1032 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.821 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.117 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.300(18) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 1176 _refine_ls_number_reflns 12321 _refine_ls_number_restraints 55 _refine_ls_restrained_S_all 1.101 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0677 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1495P)^2^+0.2603P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1937 _refine_ls_wR_factor_ref 0.2060 _reflns_Friedel_coverage 0.365 _reflns_Friedel_fraction_full 0.397 _reflns_Friedel_fraction_max 0.351 _reflns_number_gt 10349 _reflns_number_total 12321 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00948c2.cif _cod_data_source_block TCZ-SULH2 _cod_original_cell_volume 2148.82(11) _cod_database_code 7247720 _shelx_shelxl_version_number 2019/2 _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_min 0.314 _shelx_estimated_absorpt_t_max 0.897 _oxdiff_exptl_absorpt_empirical_full_min 0.497 _oxdiff_exptl_absorpt_empirical_full_max 2.167 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL AM230914a in P1 shelx.res created by SHELXL-2019/2 at 11:39:38 on 22-Sep-2023 CELL 1.54184 10.5568 10.9083 20.8988 86.078 77.368 66.240 ZERR 2.00 0.0003 0.0003 0.0004 0.002 0.002 0.003 LATT -1 SFAC C H N O S CL UNIT 64 84 8 26 6 12 MERG 2 OMIT -5 8 -9 OMIT -5 9 -7 OMIT -3 10 -2 OMIT -6 7 -12 OMIT -4 10 0 OMIT -3 10 -1 OMIT -4 10 -2 OMIT -4 10 -1 OMIT -6 8 -7 OMIT -6 7 -11 OMIT -7 7 -6 OMIT -12 -8 -12 OMIT -12 -6 -16 DFIX 0.90 0.020 O13 H13A DFIX 0.90 0.020 O13 H13B DANG 1.250 0.040 H13A O13 H13A H13B DFIX 0.90 0.020 O14 H14A DFIX 0.90 0.020 O14 H14B DANG 1.250 0.040 H14A O14 H14A H14B DFIX 0.90 0.020 O15 H15A DFIX 0.90 0.020 O15 H15B DANG 1.250 0.040 H15A O15 H15A H15B DFIX 0.90 0.020 O16 H16A DFIX 0.90 0.020 O16 H16B DANG 1.250 0.040 H16A O16 H16A H16B DFIX 0.90 0.020 O17 H17A DFIX 0.90 0.020 O17 H17B DANG 1.250 0.040 H17A O17 H17A H17B DFIX 0.90 0.020 O19 H19A DFIX 0.90 0.020 O19 H19B DANG 1.250 0.040 H19A O19 H19A H19B DFIX 0.90 0.020 O20 H20A DFIX 0.90 0.020 O20 H20B DANG 1.250 0.040 H20A O20 H20A H20B DFIX 0.90 0.020 O21 H21A DFIX 0.90 0.020 O21 H21B DANG 1.250 0.040 H21A O21 H21A H21B DFIX 0.90 0.020 O22 H22A DFIX 0.90 0.020 O22 H22B DANG 1.250 0.040 H22A O22 H22A H22B DFIX 0.90 0.020 O23 H23A DFIX 0.90 0.020 O23 H23B DANG 1.250 0.040 H23A O23 H23A H23B DFIX 0.90 0.020 O24 H24C DFIX 0.90 0.020 O24 H24D DANG 1.250 0.040 H24C O24 H24C H24D DFIX 0.90 0.020 O25 H25A DFIX 0.90 0.020 O25 H25B DANG 1.250 0.040 H25A O25 H25A H25B DFIX 0.90 0.020 O26 H26A DFIX 0.90 0.020 O26 H26B DANG 1.250 0.040 H26A O26 H26A H26B FMAP 2 PLAN 5 SIZE 0.020 0.100 0.270 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -173.00 WGHT 0.149500 0.260300 FVAR 2.27202 0.43116 0.39443 0.86550 0.89970 0.85200 C1 1 1.332452 1.040068 0.158840 11.00000 0.02807 0.02368 = 0.01984 0.00194 0.00286 -0.01064 C2 1 1.296529 1.112171 0.103633 11.00000 0.03525 0.02969 = 0.02466 0.00212 -0.00257 -0.01565 C3 1 1.392670 1.146885 0.057164 11.00000 0.04286 0.04061 = 0.01963 0.00375 0.00199 -0.02357 AFIX 43 H3 2 1.366188 1.195605 0.019411 11.00000 -1.20000 AFIX 0 C4 1 1.528081 1.107735 0.068081 11.00000 0.03400 0.04080 = 0.02687 -0.00618 0.01097 -0.02539 C5 1 1.567605 1.039238 0.122674 11.00000 0.03244 0.04879 = 0.03598 -0.00279 0.00241 -0.02455 AFIX 43 H5 2 1.660298 1.015544 0.129890 11.00000 -1.20000 AFIX 0 C6 1 1.469095 1.005220 0.167231 11.00000 0.02535 0.04223 = 0.03079 0.01066 -0.00411 -0.01744 AFIX 43 H6 2 1.496417 0.956296 0.204810 11.00000 -1.20000 AFIX 0 C7 1 1.228487 1.002848 0.209533 11.00000 0.02488 0.02418 = 0.02115 0.00497 -0.00289 -0.01059 AFIX 13 H7 2 1.136209 1.033837 0.195270 11.00000 -1.20000 AFIX 0 C8 1 1.205932 1.068785 0.275000 11.00000 0.02432 0.03000 = 0.02213 -0.00025 0.00412 -0.01591 AFIX 23 H8A 2 1.294078 1.028736 0.292061 11.00000 -1.20000 H8B 2 1.183574 1.165551 0.268910 11.00000 -1.20000 AFIX 0 C9 1 1.104281 0.969946 0.373191 11.00000 0.02324 0.02344 = 0.01939 -0.00175 -0.00252 -0.00780 AFIX 43 H9 2 1.190566 0.916039 0.386103 11.00000 -1.20000 AFIX 0 C10 1 0.877895 1.064531 0.370432 11.00000 0.02160 0.03357 = 0.02793 -0.00123 -0.00055 -0.01133 AFIX 43 H10 2 0.778658 1.087963 0.381259 11.00000 -1.20000 AFIX 0 C11 1 0.949381 1.112085 0.319524 11.00000 0.02035 0.02331 = 0.02694 0.00415 -0.00393 -0.00685 AFIX 43 H11 2 0.909498 1.174831 0.288160 11.00000 -1.20000 AFIX 0 C12 1 1.234776 0.792293 0.179341 11.00000 0.02787 0.02191 = 0.03155 -0.00516 -0.00398 -0.00816 AFIX 23 H12A 2 1.299255 0.696264 0.175576 11.00000 -1.20000 H12B 2 1.239603 0.829458 0.134736 11.00000 -1.20000 AFIX 0 C13 1 0.972052 0.863683 0.179337 11.00000 0.03292 0.02774 = 0.02985 0.00031 -0.00043 -0.01876 C14 1 1.085681 0.805443 0.207628 11.00000 0.03271 0.01929 = 0.02899 -0.00350 -0.00291 -0.01123 C15 1 1.044610 0.758788 0.271417 11.00000 0.03309 0.03258 = 0.03034 -0.00282 -0.00268 -0.01835 AFIX 43 H15 2 1.109777 0.714682 0.298884 11.00000 -1.20000 AFIX 0 C16 1 0.906951 0.782480 0.289075 11.00000 0.03347 0.03403 = 0.02774 0.00161 -0.00089 -0.02043 AFIX 43 H16 2 0.863997 0.757642 0.329814 11.00000 -1.20000 AFIX 0 C17 1 0.848595 0.522789 0.158227 11.00000 0.02982 0.03739 = 0.01722 0.00239 -0.00595 -0.02149 C18 1 0.811791 0.608553 0.107451 11.00000 0.03232 0.03085 = 0.02355 0.00212 -0.00202 -0.02002 C19 1 0.913341 0.638743 0.061479 11.00000 0.04612 0.04262 = 0.02243 0.01103 -0.00714 -0.03045 AFIX 43 H19 2 0.886699 0.698426 0.026890 11.00000 -1.20000 AFIX 0 C20 1 1.052517 0.579866 0.067655 11.00000 0.03192 0.03629 = 0.02465 -0.00288 0.00234 -0.02220 C21 1 1.092875 0.495206 0.118661 11.00000 0.03826 0.06314 = 0.03899 0.01199 -0.01121 -0.03196 AFIX 43 H21 2 1.188853 0.457129 0.122934 11.00000 -1.20000 AFIX 0 C22 1 0.990984 0.467260 0.163135 11.00000 0.03497 0.06018 = 0.03480 0.02124 -0.01355 -0.03035 AFIX 43 H22 2 1.018110 0.408744 0.198057 11.00000 -1.20000 AFIX 0 C23 1 0.741160 0.489966 0.208751 11.00000 0.02676 0.02682 = 0.02006 0.00692 -0.00678 -0.01424 AFIX 13 H23 2 0.651538 0.517686 0.192403 11.00000 -1.20000 AFIX 0 C24 1 0.710928 0.566637 0.272915 11.00000 0.02322 0.03198 = 0.01986 0.00016 0.00468 -0.01720 AFIX 23 H24A 2 0.796077 0.531106 0.292328 11.00000 -1.20000 H24B 2 0.688471 0.662555 0.263763 11.00000 -1.20000 AFIX 0 C25 1 0.601889 0.475633 0.371411 11.00000 0.02297 0.02706 = 0.01987 0.00015 -0.00341 -0.01132 AFIX 43 H25 2 0.686567 0.423568 0.386076 11.00000 -1.20000 AFIX 0 C26 1 0.377005 0.567577 0.364368 11.00000 0.02534 0.02811 = 0.03288 0.00277 -0.00052 -0.01065 AFIX 43 H26 2 0.277725 0.591283 0.373670 11.00000 -1.20000 AFIX 0 C27 1 0.452495 0.610627 0.313237 11.00000 0.02475 0.02924 = 0.02104 0.00279 -0.00355 -0.01147 AFIX 43 H27 2 0.416015 0.669111 0.279796 11.00000 -1.20000 AFIX 0 C28 1 0.745237 0.276574 0.185536 11.00000 0.02703 0.02823 = 0.03102 -0.00454 -0.00544 -0.01063 AFIX 23 H28A 2 0.807974 0.180241 0.184816 11.00000 -1.20000 H28B 2 0.752287 0.307662 0.139773 11.00000 -1.20000 AFIX 0 C29 1 0.479733 0.364113 0.187727 11.00000 0.03417 0.02179 = 0.02899 -0.00346 0.00121 -0.01635 C30 1 0.594162 0.295178 0.214678 11.00000 0.03144 0.02611 = 0.02777 -0.00470 -0.00275 -0.01774 C31 1 0.552873 0.241968 0.276471 11.00000 0.03678 0.03225 = 0.02906 0.00248 -0.00905 -0.01723 AFIX 43 H31 2 0.617802 0.189636 0.302703 11.00000 -1.20000 AFIX 0 C32 1 0.411412 0.273955 0.293747 11.00000 0.04054 0.04260 = 0.02556 0.00184 -0.00282 -0.02895 AFIX 43 H32 2 0.366707 0.246866 0.333329 11.00000 -1.20000 AFIX 0 C33 1 -0.340590 -0.038174 0.838886 11.00000 0.03034 0.03315 = 0.02317 0.00414 -0.00598 -0.02193 C34 1 -0.305827 -0.108040 0.894179 11.00000 0.03910 0.03496 = 0.02367 0.00458 -0.00574 -0.02020 C35 1 -0.400357 -0.144854 0.940267 11.00000 0.04937 0.05008 = 0.02238 0.00970 -0.00535 -0.03354 AFIX 43 H35 2 -0.371963 -0.194995 0.977391 11.00000 -1.20000 AFIX 0 C36 1 -0.535448 -0.107132 0.930901 11.00000 0.04386 0.04244 = 0.02824 -0.00222 0.00146 -0.02887 C37 1 -0.573152 -0.040030 0.874690 11.00000 0.02835 0.04590 = 0.03965 0.00583 -0.00207 -0.01693 AFIX 43 H37 2 -0.665695 -0.016986 0.867421 11.00000 -1.20000 AFIX 0 C38 1 -0.476190 -0.006782 0.829352 11.00000 0.03192 0.05295 = 0.03329 0.00649 -0.01061 -0.02160 AFIX 43 H38 2 -0.502787 0.038484 0.790860 11.00000 -1.20000 AFIX 0 C39 1 -0.238448 0.002440 0.787946 11.00000 0.02547 0.02990 = 0.01940 0.00475 -0.00337 -0.01737 AFIX 13 H39 2 -0.145774 -0.027733 0.801765 11.00000 -1.20000 AFIX 0 C40 1 -0.215589 -0.061070 0.721302 11.00000 0.03810 0.03959 = 0.02352 -0.00204 -0.00206 -0.02599 AFIX 23 H40A 2 -0.194793 -0.157760 0.726350 11.00000 -1.20000 H40B 2 -0.302867 -0.018707 0.703683 11.00000 -1.20000 AFIX 0 C41 1 -0.105427 0.042469 0.626566 11.00000 0.03256 0.03670 = 0.02330 -0.00028 -0.00781 -0.01811 AFIX 43 H41 2 -0.189873 0.103586 0.614304 11.00000 -1.20000 AFIX 0 C42 1 0.119997 -0.069259 0.628426 11.00000 0.03623 0.03045 = 0.02473 0.00283 -0.00015 -0.01720 AFIX 43 H42 2 0.220062 -0.098821 0.617100 11.00000 -1.20000 AFIX 0 C43 1 0.044173 -0.114854 0.677375 11.00000 0.02981 0.03020 = 0.02538 0.00388 -0.00167 -0.01013 AFIX 43 H43 2 0.080963 -0.182671 0.707368 11.00000 -1.20000 AFIX 0 C44 1 -0.249868 0.211261 0.822426 11.00000 0.02925 0.03821 = 0.03074 -0.01137 0.00737 -0.02055 AFIX 23 H44A 2 -0.254203 0.171390 0.866436 11.00000 -1.20000 H44B 2 -0.315375 0.306945 0.827280 11.00000 -1.20000 AFIX 0 C45 1 0.013526 0.141362 0.822425 11.00000 0.03709 0.03091 = 0.02968 -0.00648 0.00364 -0.01789 C46 1 -0.100840 0.199795 0.794241 11.00000 0.02853 0.03485 = 0.02981 -0.01078 0.00274 -0.01981 C47 1 -0.062743 0.249151 0.731135 11.00000 0.03269 0.04338 = 0.03138 -0.00252 -0.00455 -0.02383 AFIX 43 H47 2 -0.128851 0.295468 0.704393 11.00000 -1.20000 AFIX 0 C48 1 0.078119 0.223221 0.712990 11.00000 0.04425 0.04781 = 0.03066 -0.00289 -0.00625 -0.03048 AFIX 43 H48 2 0.121499 0.247587 0.672230 11.00000 -1.20000 AFIX 0 C49 1 0.141873 0.480331 0.839163 11.00000 0.02483 0.02348 = 0.02548 0.00317 -0.00481 -0.01252 C50 1 0.180471 0.391290 0.889252 11.00000 0.03936 0.02597 = 0.02093 0.00249 -0.00350 -0.01383 C51 1 0.082295 0.359642 0.935796 11.00000 0.04465 0.04980 = 0.02301 0.00682 -0.00319 -0.02641 AFIX 43 H51 2 0.110574 0.300015 0.970197 11.00000 -1.20000 AFIX 0 C52 1 -0.058262 0.418264 0.930151 11.00000 0.03602 0.03980 = 0.02628 -0.00020 0.00261 -0.02636 C53 1 -0.098292 0.503073 0.880208 11.00000 0.03596 0.06314 = 0.04261 0.01208 -0.00477 -0.03183 AFIX 43 H53 2 -0.194532 0.541189 0.876346 11.00000 -1.20000 AFIX 0 C54 1 0.002757 0.533218 0.835079 11.00000 0.03249 0.05524 = 0.03718 0.01663 -0.01174 -0.02114 AFIX 43 H54 2 -0.025852 0.592187 0.800502 11.00000 -1.20000 AFIX 0 C55 1 0.251507 0.513708 0.788996 11.00000 0.02570 0.02550 = 0.02128 0.00106 0.00478 -0.01558 AFIX 13 H55 2 0.340378 0.486983 0.805878 11.00000 -1.20000 AFIX 0 C56 1 0.283116 0.439246 0.724637 11.00000 0.03734 0.02701 = 0.02853 0.00046 -0.00452 -0.01863 AFIX 23 H56A 2 0.304910 0.343215 0.733147 11.00000 -1.20000 H56B 2 0.198768 0.475759 0.704651 11.00000 -1.20000 AFIX 0 C57 1 0.399056 0.533020 0.627751 11.00000 0.03042 0.02790 = 0.02514 0.00033 -0.00683 -0.01307 AFIX 43 H57 2 0.315730 0.590349 0.613335 11.00000 -1.20000 AFIX 0 C58 1 0.621137 0.430821 0.634579 11.00000 0.03095 0.03592 = 0.02605 0.00018 -0.00349 -0.01606 AFIX 43 H58 2 0.720792 0.404688 0.625513 11.00000 -1.20000 AFIX 0 C59 1 0.544078 0.387041 0.683904 11.00000 0.02503 0.02646 = 0.03004 0.00583 -0.00514 -0.00843 AFIX 43 H59 2 0.579528 0.323236 0.715730 11.00000 -1.20000 AFIX 0 C60 1 0.240228 0.728483 0.815585 11.00000 0.03047 0.03362 = 0.03224 -0.00754 0.00162 -0.01962 AFIX 23 H60A 2 0.232150 0.696460 0.861177 11.00000 -1.20000 H60B 2 0.176473 0.824539 0.816492 11.00000 -1.20000 AFIX 0 C61 1 0.504550 0.640960 0.814515 11.00000 0.02995 0.03743 = 0.03099 -0.00327 0.00220 -0.02048 C62 1 0.388855 0.712116 0.788107 11.00000 0.03188 0.03132 = 0.02564 -0.00629 -0.00026 -0.01688 C63 1 0.430450 0.766891 0.726437 11.00000 0.03907 0.04593 = 0.02617 -0.00446 -0.00346 -0.02937 AFIX 43 H63 2 0.365620 0.821286 0.700604 11.00000 -1.20000 AFIX 0 C64 1 0.573595 0.732187 0.708963 11.00000 0.03699 0.04817 = 0.02955 -0.00214 -0.00305 -0.02712 AFIX 43 H64 2 0.619289 0.758117 0.669310 11.00000 -1.20000 AFIX 0 N1 3 0.975919 0.976758 0.402973 11.00000 0.03059 0.03441 = 0.01828 0.00411 -0.00117 -0.01835 AFIX 43 H1N 2 0.957443 0.932003 0.437881 11.00000 -1.20000 AFIX 0 N2 3 1.090896 1.051575 0.322276 11.00000 0.02532 0.02527 = 0.01829 0.00211 0.00141 -0.01387 N3 3 0.471826 0.483374 0.399891 11.00000 0.03260 0.02833 = 0.01983 0.00223 -0.00181 -0.01837 AFIX 43 H3N 2 0.450777 0.441422 0.435455 11.00000 -1.20000 AFIX 0 N4 3 0.592195 0.553017 0.319296 11.00000 0.02321 0.02581 = 0.01818 0.00271 -0.00049 -0.01060 N5 3 -0.097982 -0.043707 0.675553 11.00000 0.02524 0.03130 = 0.01802 -0.00118 -0.00103 -0.01603 N6 3 0.023029 0.028561 0.598336 11.00000 0.04430 0.03230 = 0.01872 0.00188 -0.00576 -0.02287 N7 3 0.403415 0.453067 0.679163 11.00000 0.02684 0.02840 = 0.02251 0.00052 -0.00152 -0.01636 N8 3 0.527899 0.519883 0.600335 11.00000 0.04177 0.03006 = 0.02103 0.00108 -0.00454 -0.02045 O1 4 1.280659 0.860876 0.219129 11.00000 0.02345 0.02326 = 0.02838 0.00414 -0.00432 -0.01265 O2 4 0.790647 0.350429 0.223089 11.00000 0.02892 0.02980 = 0.02571 0.00425 -0.00756 -0.01805 O3 4 -0.293227 0.143322 0.780243 11.00000 0.02875 0.02796 = 0.02661 0.00335 -0.00560 -0.01235 O4 4 0.197887 0.653625 0.776342 11.00000 0.02770 0.02565 = 0.02733 0.00375 -0.00543 -0.01392 O5 4 0.920366 0.862270 0.517379 11.00000 0.02380 0.02979 = 0.03122 0.00283 -0.00597 -0.01566 O6 4 0.666027 0.941587 0.551862 11.00000 0.02560 0.03126 = 0.11468 0.00219 -0.00669 -0.01033 O7 4 0.810620 0.721457 0.579603 11.00000 0.04525 0.03483 = 0.03031 0.00930 -0.00691 -0.02131 O8A 4 0.778561 0.786274 0.470067 21.00000 0.01335 O8B 4 0.807181 0.748502 0.466667 -21.00000 0.05265 O9 4 0.423812 0.360157 0.511574 11.00000 0.02805 0.02797 = 0.03107 0.00686 -0.00719 -0.01579 O10A 4 0.264675 0.311820 0.596060 31.00000 0.03309 O10B 4 0.295682 0.236082 0.578562 -31.00000 0.03034 O11A 4 0.331331 0.198398 0.492044 31.00000 0.03307 O11B 4 0.320330 0.235586 0.463335 -31.00000 0.04398 O12A 4 0.178377 0.434539 0.506052 31.00000 0.01083 O12B 4 0.166747 0.440186 0.530877 -31.00000 0.05664 O13 4 0.985900 0.600112 0.666325 11.00000 0.12349 0.06381 = 0.08549 0.02492 -0.07705 -0.05001 O14 4 0.394411 0.955316 0.549452 11.00000 0.02538 0.02959 = 0.03712 -0.00024 -0.00228 -0.01272 O15 4 0.895691 0.451937 0.551763 11.00000 0.02622 0.03085 = 0.04598 -0.00384 -0.00239 -0.01366 O16 4 0.859633 0.314197 0.454269 11.00000 0.02970 0.02837 = 0.03478 -0.00151 -0.00203 -0.01371 O17 4 0.614849 0.628124 0.486868 11.00000 0.02893 0.03117 = 0.02788 0.00676 -0.00585 -0.01798 O18 4 0.364247 0.807284 0.453874 11.00000 0.03390 0.03545 = 0.02863 -0.00177 -0.00222 -0.01888 O19 4 0.512349 0.878646 0.330518 11.00000 0.04127 0.04049 = 0.02584 0.00171 -0.00667 -0.01952 O20 4 0.693642 0.189256 0.523486 11.00000 0.02082 0.02390 = 0.03863 0.00137 -0.00777 -0.00981 O21 4 0.195413 0.686325 0.523096 11.00000 0.01781 0.02649 = 0.04278 -0.00153 -0.00773 -0.00642 O22 4 0.471669 0.117467 0.665717 11.00000 0.07497 0.04806 = 0.04009 0.01045 -0.02788 -0.02931 O23 4 0.057609 0.566456 0.406333 11.00000 0.04096 0.05511 = 0.03205 -0.00382 -0.00025 -0.03166 O24 4 0.582243 0.031273 0.408576 11.00000 0.03653 0.05936 = 0.02922 0.00020 -0.00212 -0.03015 O25 4 0.013024 0.382706 0.333144 11.00000 0.04844 0.03902 = 0.02698 0.00009 -0.00493 -0.02446 O26 4 0.113435 0.131221 0.483904 11.00000 0.02783 0.03016 = 0.02601 0.00595 -0.00466 -0.01760 S1 5 0.817704 0.863434 0.228826 11.00000 0.02769 0.03714 = 0.03584 0.00469 -0.00225 -0.01925 S2 5 0.322980 0.368120 0.236507 11.00000 0.02930 0.03651 = 0.03172 -0.00042 -0.00104 -0.01973 S3 5 0.167645 0.140364 0.773621 11.00000 0.03382 0.04117 = 0.03386 -0.00175 0.00197 -0.02364 S4 5 0.661813 0.635542 0.767488 11.00000 0.03113 0.04465 = 0.03543 -0.00307 0.00144 -0.02305 S5 5 0.796548 0.823187 0.530206 11.00000 0.01936 0.02225 = 0.02823 0.00563 -0.00448 -0.00967 S6 5 0.299970 0.321247 0.524096 11.00000 0.02018 0.02467 = 0.03076 0.00971 -0.00518 -0.01055 CL1A 6 1.127712 1.155812 0.086983 41.00000 0.03724 0.05058 = 0.03077 0.01703 -0.01528 -0.02518 CL1B 6 1.129319 1.198033 0.104425 -41.00000 0.03372 CL2 6 1.651317 1.148074 0.011630 11.00000 0.05253 0.06312 = 0.02887 -0.00502 0.01147 -0.04164 CL3 6 0.969494 0.928876 0.103008 11.00000 0.03457 0.03919 = 0.03521 0.00942 -0.00294 -0.01652 CL4 6 0.638332 0.685712 0.100820 11.00000 0.03407 0.05055 = 0.05007 0.02968 -0.00721 -0.01161 CL5A 6 1.182805 0.611385 0.011329 51.00000 0.03806 0.05312 = 0.02698 0.00428 0.00608 -0.02967 CL5B 6 1.136298 0.670565 0.011108 -51.00000 0.04356 CL6 6 0.478691 0.441003 0.114068 11.00000 0.03282 0.03233 = 0.03014 0.00430 -0.00202 -0.01322 CL7 6 -0.135412 -0.158198 0.910061 11.00000 0.04166 0.06232 = 0.03954 0.02512 -0.01573 -0.02727 CL8 6 -0.658701 -0.147254 0.987859 11.00000 0.05878 0.07459 = 0.03218 -0.00351 0.01007 -0.05009 CL9 6 0.020128 0.069923 0.899348 11.00000 0.04171 0.04075 = 0.03433 0.00342 0.00108 -0.02054 CL1C 6 0.358271 0.307208 0.894867 61.00000 0.02985 0.03638 = 0.04619 0.02083 -0.00665 -0.01005 CL1D 6 0.349736 0.355598 0.913105 -61.00000 0.04714 CL11 6 -0.184386 0.382377 0.987777 11.00000 0.04601 0.05919 = 0.03274 -0.00030 0.00693 -0.03480 CL12 6 0.507357 0.558294 0.888704 11.00000 0.03626 0.03852 = 0.03738 0.00611 -0.00112 -0.01653 H6N 2 0.052124 0.054298 0.565539 11.00000 0.05795 H8N 2 0.551458 0.563984 0.572395 11.00000 0.04476 H13A 2 0.998140 0.532346 0.635465 11.00000 0.07709 H13B 2 0.930803 0.659772 0.642090 11.00000 0.05423 H14A 2 0.364757 1.045616 0.565259 11.00000 0.05895 H14B 2 0.481575 0.945443 0.552337 11.00000 0.03873 H15A 2 0.872583 0.546745 0.546321 11.00000 0.13636 H15B 2 0.983229 0.442909 0.550010 11.00000 0.02697 H16A 2 0.767977 0.380247 0.474558 11.00000 0.08449 H16B 2 0.819164 0.254898 0.464722 11.00000 0.05383 H17A 2 0.669877 0.681312 0.484686 11.00000 -1.20000 H17B 2 0.560104 0.693814 0.464613 11.00000 0.03406 H18A 2 0.274305 0.886786 0.467548 11.00000 0.08084 H18B 2 0.313628 0.758223 0.467381 11.00000 0.03067 H19A 2 0.479151 0.837676 0.369145 11.00000 0.04185 H19B 2 0.537784 0.919710 0.358099 11.00000 0.05698 H20A 2 0.597230 0.243005 0.520335 11.00000 0.04694 H20B 2 0.680568 0.128435 0.501546 11.00000 0.08321 H21A 2 0.174050 0.630634 0.496971 11.00000 0.09898 H21B 2 0.103967 0.737864 0.529763 11.00000 0.01670 H22A 2 0.518426 0.053891 0.629737 11.00000 0.06530 H22B 2 0.418889 0.171722 0.638902 11.00000 0.05812 H23A 2 0.096822 0.497577 0.435338 11.00000 0.01539 H23B 2 -0.014577 0.610820 0.438564 11.00000 0.07566 H24C 2 0.602203 -0.011094 0.449603 11.00000 0.20257 H24D 2 0.500946 0.086704 0.433525 11.00000 0.03977 H25A 2 -0.022439 0.346863 0.373316 11.00000 0.06899 H25B 2 0.051815 0.412898 0.359363 11.00000 0.05867 H26A 2 0.174080 0.180002 0.476327 11.00000 -1.20000 H26B 2 0.052880 0.205282 0.468321 11.00000 0.04290 HKLF 4 REM AM230914a in P1 REM wR2 = 0.2060, GooF = S = 1.069, Restrained GooF = 1.101 for all data REM R1 = 0.0677 for 10349 Fo > 4sig(Fo) and 0.0773 for all 12321 data REM 1176 parameters refined using 55 restraints END WGHT 0.1495 0.2603 REM Highest difference peak 0.821, deepest hole -0.690, 1-sigma level 0.117 Q1 1 0.7195 0.9056 0.5051 11.00000 0.05 0.82 Q2 1 0.2661 0.3004 0.4733 11.00000 0.05 0.79 Q3 1 0.7610 0.8194 0.5962 11.00000 0.05 0.72 Q4 1 1.1173 0.6751 -0.0092 11.00000 0.05 0.68 Q5 1 0.5088 0.5970 0.9112 11.00000 0.05 0.67 ; _shelx_res_checksum 86500 loop_ _space_group_symop_operation_xyz '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 C1 C 1.3325(7) 1.0401(7) 0.1588(3) 0.0251(13) Uani 1 1 d . . . . . C2 C 1.2965(8) 1.1122(8) 0.1036(3) 0.0297(15) Uani 1 1 d . . . . . C3 C 1.3927(9) 1.1469(8) 0.0572(3) 0.0337(16) Uani 1 1 d . . . . . H3 H 1.366188 1.195605 0.019411 0.040 Uiso 1 1 calc R U . . . C4 C 1.5281(8) 1.1077(8) 0.0681(3) 0.0330(17) Uani 1 1 d . . . . . C5 C 1.5676(9) 1.0392(9) 0.1227(4) 0.0377(18) Uani 1 1 d . . . . . H5 H 1.660298 1.015544 0.129890 0.045 Uiso 1 1 calc R U . . . C6 C 1.4691(8) 1.0052(8) 0.1672(4) 0.0323(16) Uani 1 1 d . . . . . H6 H 1.496417 0.956296 0.204810 0.039 Uiso 1 1 calc R U . . . C7 C 1.2285(7) 1.0028(7) 0.2095(3) 0.0237(13) Uani 1 1 d . . . . . H7 H 1.136209 1.033837 0.195270 0.028 Uiso 1 1 calc R U . . . C8 C 1.2059(7) 1.0688(7) 0.2750(3) 0.0253(13) Uani 1 1 d . . . . . H8A H 1.294078 1.028736 0.292061 0.030 Uiso 1 1 calc R U . . . H8B H 1.183574 1.165551 0.268910 0.030 Uiso 1 1 calc R U . . . C9 C 1.1043(7) 0.9699(7) 0.3732(3) 0.0227(12) Uani 1 1 d . . . . . H9 H 1.190566 0.916039 0.386103 0.027 Uiso 1 1 calc R U . . . C10 C 0.8779(7) 1.0645(8) 0.3704(3) 0.0283(14) Uani 1 1 d . . . . . H10 H 0.778658 1.087963 0.381259 0.034 Uiso 1 1 calc R U . . . C11 C 0.9494(7) 1.1121(7) 0.3195(3) 0.0245(13) Uani 1 1 d . . . . . H11 H 0.909498 1.174831 0.288160 0.029 Uiso 1 1 calc R U . . . C12 C 1.2348(8) 0.7923(7) 0.1793(3) 0.0278(14) Uani 1 1 d . . . . . H12A H 1.299255 0.696264 0.175576 0.033 Uiso 1 1 calc R U . . . H12B H 1.239603 0.829458 0.134736 0.033 Uiso 1 1 calc R U . . . C13 C 0.9721(8) 0.8637(7) 0.1793(3) 0.0290(14) Uani 1 1 d . . . . . C14 C 1.0857(8) 0.8054(7) 0.2076(3) 0.0271(14) Uani 1 1 d . . . . . C15 C 1.0446(8) 0.7588(8) 0.2714(4) 0.0308(15) Uani 1 1 d . . . . . H15 H 1.109777 0.714682 0.298884 0.037 Uiso 1 1 calc R U . . . C16 C 0.9070(8) 0.7825(8) 0.2891(3) 0.0304(14) Uani 1 1 d . . . . . H16 H 0.863997 0.757642 0.329814 0.037 Uiso 1 1 calc R U . . . C17 C 0.8486(7) 0.5228(7) 0.1582(3) 0.0254(14) Uani 1 1 d . . . . . C18 C 0.8118(8) 0.6086(7) 0.1075(3) 0.0272(14) Uani 1 1 d . . . . . C19 C 0.9133(9) 0.6387(8) 0.0615(3) 0.0334(16) Uani 1 1 d . . . . . H19 H 0.886699 0.698426 0.026890 0.040 Uiso 1 1 calc R U . . . C20 C 1.0525(8) 0.5799(8) 0.0677(3) 0.0293(15) Uani 1 1 d . . . . . C21 C 1.0929(9) 0.4952(10) 0.1187(4) 0.043(2) Uani 1 1 d . . . . . H21 H 1.188853 0.457129 0.122934 0.052 Uiso 1 1 calc R U . . . C22 C 0.9910(9) 0.4673(10) 0.1631(4) 0.0396(19) Uani 1 1 d . . . . . H22 H 1.018110 0.408744 0.198057 0.047 Uiso 1 1 calc R U . . . C23 C 0.7412(7) 0.4900(7) 0.2088(3) 0.0234(13) Uani 1 1 d . . . . . H23 H 0.651538 0.517686 0.192403 0.028 Uiso 1 1 calc R U . . . C24 C 0.7109(7) 0.5666(7) 0.2729(3) 0.0245(13) Uani 1 1 d . . . . . H24A H 0.796077 0.531106 0.292328 0.029 Uiso 1 1 calc R U . . . H24B H 0.688471 0.662555 0.263763 0.029 Uiso 1 1 calc R U . . . C25 C 0.6019(7) 0.4756(7) 0.3714(3) 0.0230(12) Uani 1 1 d . . . . . H25 H 0.686567 0.423568 0.386076 0.028 Uiso 1 1 calc R U . . . C26 C 0.3770(8) 0.5676(8) 0.3644(4) 0.0298(14) Uani 1 1 d . . . . . H26 H 0.277725 0.591283 0.373670 0.036 Uiso 1 1 calc R U . . . C27 C 0.4525(7) 0.6106(7) 0.3132(3) 0.0251(13) Uani 1 1 d . . . . . H27 H 0.416015 0.669111 0.279796 0.030 Uiso 1 1 calc R U . . . C28 C 0.7452(8) 0.2766(8) 0.1855(4) 0.0287(14) Uani 1 1 d . . . . . H28A H 0.807974 0.180241 0.184816 0.034 Uiso 1 1 calc R U . . . H28B H 0.752287 0.307662 0.139773 0.034 Uiso 1 1 calc R U . . . C29 C 0.4797(8) 0.3641(7) 0.1877(3) 0.0277(14) Uani 1 1 d . . . . . C30 C 0.5942(8) 0.2952(7) 0.2147(3) 0.0267(14) Uani 1 1 d . . . . . C31 C 0.5529(8) 0.2420(8) 0.2765(3) 0.0313(15) Uani 1 1 d . . . . . H31 H 0.617802 0.189636 0.302703 0.038 Uiso 1 1 calc R U . . . C32 C 0.4114(9) 0.2740(8) 0.2937(3) 0.0329(16) Uani 1 1 d . . . . . H32 H 0.366707 0.246866 0.333329 0.039 Uiso 1 1 calc R U . . . C33 C -0.3406(8) -0.0382(7) 0.8389(3) 0.0260(14) Uani 1 1 d . . . . . C34 C -0.3058(8) -0.1080(8) 0.8942(3) 0.0311(15) Uani 1 1 d . . . . . C35 C -0.4004(9) -0.1449(9) 0.9403(3) 0.0369(17) Uani 1 1 d . . . . . H35 H -0.371963 -0.194995 0.977391 0.044 Uiso 1 1 calc R U . . . C36 C -0.5354(9) -0.1071(9) 0.9309(4) 0.0357(17) Uani 1 1 d . . . . . C37 C -0.5732(9) -0.0400(9) 0.8747(4) 0.0384(18) Uani 1 1 d . . . . . H37 H -0.665695 -0.016986 0.867421 0.046 Uiso 1 1 calc R U . . . C38 C -0.4762(9) -0.0068(9) 0.8294(4) 0.0375(17) Uani 1 1 d . . . . . H38 H -0.502787 0.038484 0.790860 0.045 Uiso 1 1 calc R U . . . C39 C -0.2384(7) 0.0024(7) 0.7879(3) 0.0233(13) Uani 1 1 d . . . . . H39 H -0.145774 -0.027733 0.801765 0.028 Uiso 1 1 calc R U . . . C40 C -0.2156(8) -0.0611(8) 0.7213(3) 0.0309(15) Uani 1 1 d . . . . . H40A H -0.194793 -0.157760 0.726350 0.037 Uiso 1 1 calc R U . . . H40B H -0.302867 -0.018707 0.703683 0.037 Uiso 1 1 calc R U . . . C41 C -0.1054(8) 0.0425(8) 0.6266(3) 0.0291(14) Uani 1 1 d . . . . . H41 H -0.189873 0.103586 0.614304 0.035 Uiso 1 1 calc R U . . . C42 C 0.1200(8) -0.0693(7) 0.6284(3) 0.0303(15) Uani 1 1 d . . . . . H42 H 0.220062 -0.098821 0.617100 0.036 Uiso 1 1 calc R U . . . C43 C 0.0442(8) -0.1149(8) 0.6774(3) 0.0299(15) Uani 1 1 d . . . . . H43 H 0.080963 -0.182671 0.707368 0.036 Uiso 1 1 calc R U . . . C44 C -0.2499(8) 0.2113(8) 0.8224(4) 0.0321(16) Uani 1 1 d . . . . . H44A H -0.254203 0.171390 0.866436 0.038 Uiso 1 1 calc R U . . . H44B H -0.315375 0.306945 0.827280 0.038 Uiso 1 1 calc R U . . . C45 C 0.0135(9) 0.1414(8) 0.8224(4) 0.0325(15) Uani 1 1 d . . . . . C46 C -0.1008(8) 0.1998(8) 0.7942(3) 0.0296(15) Uani 1 1 d . . . . . C47 C -0.0627(8) 0.2492(8) 0.7311(4) 0.0332(16) Uani 1 1 d . . . . . H47 H -0.128851 0.295468 0.704393 0.040 Uiso 1 1 calc R U . . . C48 C 0.0781(9) 0.2232(9) 0.7130(4) 0.0370(17) Uani 1 1 d . . . . . H48 H 0.121499 0.247587 0.672230 0.044 Uiso 1 1 calc R U . . . C49 C 0.1419(7) 0.4803(7) 0.8392(3) 0.0239(13) Uani 1 1 d . . . . . C50 C 0.1805(8) 0.3913(7) 0.8893(3) 0.0291(15) Uani 1 1 d . . . . . C51 C 0.0823(10) 0.3596(9) 0.9358(4) 0.0376(18) Uani 1 1 d . . . . . H51 H 0.110574 0.300015 0.970197 0.045 Uiso 1 1 calc R U . . . C52 C -0.0583(8) 0.4183(8) 0.9302(3) 0.0318(16) Uani 1 1 d . . . . . C53 C -0.0983(10) 0.5031(10) 0.8802(4) 0.044(2) Uani 1 1 d . . . . . H53 H -0.194532 0.541189 0.876346 0.053 Uiso 1 1 calc R U . . . C54 C 0.0028(9) 0.5332(10) 0.8351(4) 0.0405(19) Uani 1 1 d . . . . . H54 H -0.025852 0.592187 0.800502 0.049 Uiso 1 1 calc R U . . . C55 C 0.2515(7) 0.5137(7) 0.7890(3) 0.0240(13) Uani 1 1 d . . . . . H55 H 0.340378 0.486983 0.805878 0.029 Uiso 1 1 calc R U . . . C56 C 0.2831(8) 0.4392(7) 0.7246(3) 0.0294(15) Uani 1 1 d . . . . . H56A H 0.304910 0.343215 0.733147 0.035 Uiso 1 1 calc R U . . . H56B H 0.198768 0.475759 0.704651 0.035 Uiso 1 1 calc R U . . . C57 C 0.3991(8) 0.5330(7) 0.6278(3) 0.0272(14) Uani 1 1 d . . . . . H57 H 0.315730 0.590349 0.613335 0.033 Uiso 1 1 calc R U . . . C58 C 0.6211(8) 0.4308(8) 0.6346(3) 0.0305(15) Uani 1 1 d . . . . . H58 H 0.720792 0.404688 0.625513 0.037 Uiso 1 1 calc R U . . . C59 C 0.5441(8) 0.3870(7) 0.6839(3) 0.0281(14) Uani 1 1 d . . . . . H59 H 0.579528 0.323236 0.715730 0.034 Uiso 1 1 calc R U . . . C60 C 0.2402(8) 0.7285(8) 0.8156(4) 0.0308(15) Uani 1 1 d . . . . . H60A H 0.232150 0.696460 0.861177 0.037 Uiso 1 1 calc R U . . . H60B H 0.176473 0.824539 0.816492 0.037 Uiso 1 1 calc R U . . . C61 C 0.5046(8) 0.6410(8) 0.8145(4) 0.0317(15) Uani 1 1 d . . . . . C62 C 0.3889(8) 0.7121(7) 0.7881(3) 0.0288(14) Uani 1 1 d . . . . . C63 C 0.4304(9) 0.7669(8) 0.7264(3) 0.0333(16) Uani 1 1 d . . . . . H63 H 0.365620 0.821286 0.700604 0.040 Uiso 1 1 calc R U . . . C64 C 0.5736(9) 0.7322(9) 0.7090(4) 0.0354(16) Uani 1 1 d . . . . . H64 H 0.619289 0.758117 0.669310 0.042 Uiso 1 1 calc R U . . . N1 N 0.9759(6) 0.9768(6) 0.4030(3) 0.0268(12) Uani 1 1 d . . . . . H1N H 0.957443 0.932003 0.437881 0.032 Uiso 1 1 calc R U . . . N2 N 1.0909(6) 1.0516(6) 0.3223(3) 0.0228(11) Uani 1 1 d . . . . . N3 N 0.4718(7) 0.4834(6) 0.3999(3) 0.0256(12) Uani 1 1 d . . . . . H3N H 0.450777 0.441422 0.435455 0.031 Uiso 1 1 calc R U . . . N4 N 0.5922(6) 0.5530(6) 0.3193(3) 0.0229(11) Uani 1 1 d . . . . . N5 N -0.0980(6) -0.0437(6) 0.6756(3) 0.0238(11) Uani 1 1 d . . . . . N6 N 0.0230(7) 0.0286(6) 0.5983(3) 0.0295(13) Uani 1 1 d . . . . . N7 N 0.4034(6) 0.4531(6) 0.6792(3) 0.0248(11) Uani 1 1 d . . . . . N8 N 0.5279(7) 0.5199(7) 0.6003(3) 0.0293(12) Uani 1 1 d . . . . . O1 O 1.2807(5) 0.8609(5) 0.2191(2) 0.0243(9) Uani 1 1 d . . . . . O2 O 0.7906(5) 0.3504(5) 0.2231(2) 0.0259(10) Uani 1 1 d . . . . . O3 O -0.2932(5) 0.1433(5) 0.7802(2) 0.0276(10) Uani 1 1 d . . . . . O4 O 0.1979(5) 0.6536(5) 0.7763(2) 0.0260(10) Uani 1 1 d . . . . . O5 O 0.9204(5) 0.8623(5) 0.5174(2) 0.0267(9) Uani 1 1 d . . . . . O6 O 0.6660(6) 0.9416(6) 0.5519(4) 0.0589(19) Uani 1 1 d . . . . . O7 O 0.8106(6) 0.7215(5) 0.5796(2) 0.0356(10) Uani 1 1 d . . . . . O8A O 0.7786(19) 0.786(2) 0.4701(5) 0.013(5) Uiso 0.43(8) 1 d . . P . . O8B O 0.807(3) 0.749(4) 0.4667(8) 0.053(4) Uiso 0.57(8) 1 d . . P . . O9 O 0.4238(5) 0.3602(5) 0.5116(2) 0.0277(10) Uani 1 1 d . . . . . O10A O 0.2647(13) 0.3118(13) 0.5961(6) 0.033(3) Uiso 0.394(15) 1 d . . P . . O10B O 0.2957(8) 0.2361(9) 0.5786(4) 0.030(2) Uiso 0.606(15) 1 d . . P . . O11A O 0.3313(13) 0.1984(13) 0.4920(7) 0.033(3) Uiso 0.394(15) 1 d . . P . . O11B O 0.3203(10) 0.2356(11) 0.4633(5) 0.044(2) Uiso 0.606(15) 1 d . . P . . O12A O 0.1784(9) 0.4345(9) 0.5061(5) 0.011(2) Uiso 0.394(15) 1 d . . P . . O12B O 0.1667(13) 0.4402(12) 0.5309(8) 0.057(3) Uiso 0.606(15) 1 d . . P . . O13 O 0.9859(12) 0.6001(9) 0.6663(5) 0.079(3) Uani 1 1 d D . . . . O14 O 0.3944(5) 0.9553(5) 0.5495(2) 0.0308(10) Uani 1 1 d D . . . . O15 O 0.8957(5) 0.4519(5) 0.5518(3) 0.0342(10) Uani 1 1 d D . . . . O16 O 0.8596(5) 0.3142(5) 0.4543(2) 0.0309(10) Uani 1 1 d D . . . . O17 O 0.6148(5) 0.6281(5) 0.4869(2) 0.0277(10) Uani 1 1 d D . . . . O18 O 0.3642(6) 0.8073(5) 0.4539(2) 0.0316(10) Uani 1 1 d . . . . . O19 O 0.5123(6) 0.8786(6) 0.3305(2) 0.0349(12) Uani 1 1 d D . . . . O20 O 0.6936(5) 0.1893(5) 0.5235(2) 0.0273(9) Uani 1 1 d D . . . . O21 O 0.1954(5) 0.6863(5) 0.5231(3) 0.0295(9) Uani 1 1 d D . . . . O22 O 0.4717(9) 0.1175(7) 0.6657(3) 0.0506(16) Uani 1 1 d D . . . . O23 O 0.0576(6) 0.5665(6) 0.4063(2) 0.0396(12) Uani 1 1 d D . . . . O24 O 0.5822(6) 0.0313(6) 0.4086(2) 0.0388(12) Uani 1 1 d D . . . . O25 O 0.0130(7) 0.3827(6) 0.3331(2) 0.0363(12) Uani 1 1 d D . . . . O26 O 0.1134(5) 0.1312(5) 0.4839(2) 0.0265(9) Uani 1 1 d D . . . . S1 S 0.81770(19) 0.86343(19) 0.22883(9) 0.0324(4) Uani 1 1 d . . . . . S2 S 0.32298(19) 0.36812(19) 0.23651(8) 0.0312(4) Uani 1 1 d . . . . . S3 S 0.1676(2) 0.1404(2) 0.77362(9) 0.0348(4) Uani 1 1 d . . . . . S4 S 0.6618(2) 0.6355(2) 0.76749(9) 0.0357(4) Uani 1 1 d . . . . . S5 S 0.79655(15) 0.82319(15) 0.53021(7) 0.0232(3) Uani 1 1 d . . . . . S6 S 0.29997(15) 0.32125(16) 0.52410(7) 0.0252(3) Uani 1 1 d . . . . . Cl1A Cl 1.1277(2) 1.1558(4) 0.08698(17) 0.0365(11) Uani 0.865(18) 1 d . . P . . Cl1B Cl 1.1293(17) 1.198(2) 0.1044(11) 0.034(5) Uiso 0.135(18) 1 d . . P . . Cl2 Cl 1.6513(2) 1.1481(2) 0.01163(9) 0.0451(5) Uani 1 1 d . . . . . Cl3 Cl 0.9695(2) 0.9289(2) 0.10301(9) 0.0369(4) Uani 1 1 d . . . . . Cl4 Cl 0.6383(2) 0.6857(2) 0.10082(11) 0.0483(6) Uani 1 1 d . . . . . Cl5A Cl 1.1828(4) 0.6114(5) 0.01133(10) 0.0379(11) Uani 0.900(17) 1 d . . P . . Cl5B Cl 1.136(4) 0.671(4) 0.0111(11) 0.044(6) Uiso 0.100(17) 1 d . . P . . Cl6 Cl 0.47869(19) 0.44100(18) 0.11407(8) 0.0326(4) Uani 1 1 d . . . . . Cl7 Cl -0.1354(2) -0.1582(3) 0.91006(10) 0.0457(5) Uani 1 1 d . . . . . Cl8 Cl -0.6587(3) -0.1473(3) 0.98786(10) 0.0505(6) Uani 1 1 d . . . . . Cl9 Cl 0.0201(2) 0.0699(2) 0.89935(9) 0.0392(5) Uani 1 1 d . . . . . Cl1C Cl 0.3583(3) 0.3072(4) 0.8949(2) 0.0397(13) Uani 0.852(18) 1 d . . P . . Cl1D Cl 0.350(2) 0.356(3) 0.9131(10) 0.047(5) Uiso 0.148(18) 1 d . . P . . Cl11 Cl -0.1844(2) 0.3824(2) 0.98778(9) 0.0439(5) Uani 1 1 d . . . . . Cl12 Cl 0.5074(2) 0.5583(2) 0.88870(9) 0.0382(4) Uani 1 1 d . . . . . H6N H 0.052(12) 0.054(12) 0.566(6) 0.06(3) Uiso 1 1 d . . . . . H8N H 0.551(11) 0.564(11) 0.572(5) 0.04(3) Uiso 1 1 d . . . . . H13A H 0.998(13) 0.532(7) 0.635(5) 0.08(4) Uiso 1 1 d D . . . . H13B H 0.931(10) 0.660(7) 0.642(4) 0.05(3) Uiso 1 1 d D . . . . H14A H 0.365(9) 1.046(4) 0.565(5) 0.06(3) Uiso 1 1 d D . . . . H14B H 0.482(4) 0.945(8) 0.552(5) 0.04(2) Uiso 1 1 d D . . . . H15A H 0.873(12) 0.547(3) 0.546(9) 0.14(7) Uiso 1 1 d D . . . . H15B H 0.983(4) 0.443(8) 0.550(4) 0.027(19) Uiso 1 1 d D . . . . H16A H 0.768(7) 0.380(8) 0.475(7) 0.08(4) Uiso 1 1 d D . . . . H16B H 0.819(10) 0.255(8) 0.465(5) 0.05(3) Uiso 1 1 d D . . . . H17A H 0.670(9) 0.681(9) 0.485(6) 0.065 Uiso 1 1 d D U . . . H17B H 0.560(8) 0.694(6) 0.465(4) 0.03(2) Uiso 1 1 d D . . . . H18A H 0.274(14) 0.887(14) 0.468(7) 0.08(4) Uiso 1 1 d . . . . . H18B H 0.314(9) 0.758(9) 0.467(4) 0.03(2) Uiso 1 1 d . . . . . H19A H 0.479(10) 0.838(9) 0.369(3) 0.04(2) Uiso 1 1 d D . . . . H19B H 0.538(11) 0.920(10) 0.358(4) 0.06(3) Uiso 1 1 d D . . . . H20A H 0.597(4) 0.243(8) 0.520(5) 0.05(3) Uiso 1 1 d D . . . . H20B H 0.681(11) 0.128(8) 0.502(7) 0.08(4) Uiso 1 1 d D . . . . H21A H 0.174(10) 0.631(11) 0.497(7) 0.10(5) Uiso 1 1 d D . . . . H21B H 0.104(3) 0.738(6) 0.530(3) 0.017(17) Uiso 1 1 d D . . . . H22A H 0.518(11) 0.054(8) 0.630(4) 0.07(3) Uiso 1 1 d D . . . . H22B H 0.419(10) 0.172(8) 0.639(4) 0.06(3) Uiso 1 1 d D . . . . H23A H 0.097(7) 0.498(5) 0.435(3) 0.015(16) Uiso 1 1 d D . . . . H23B H -0.015(8) 0.611(9) 0.439(3) 0.08(4) Uiso 1 1 d D . . . . H24C H 0.602(17) -0.011(19) 0.450(4) 0.20(11) Uiso 1 1 d D . . . . H24D H 0.501(6) 0.087(8) 0.434(4) 0.04(2) Uiso 1 1 d D . . . . H25A H -0.022(12) 0.347(11) 0.373(3) 0.07(3) Uiso 1 1 d D . . . . H25B H 0.052(11) 0.413(11) 0.359(4) 0.06(3) Uiso 1 1 d D . . . . H26A H 0.174(9) 0.180(9) 0.476(6) 0.070 Uiso 1 1 d D U . . . H26B H 0.053(8) 0.205(6) 0.468(4) 0.04(2) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(3) 0.024(3) 0.020(3) 0.002(2) 0.003(2) -0.011(3) C2 0.035(4) 0.030(4) 0.025(3) 0.002(3) -0.003(3) -0.016(3) C3 0.043(4) 0.041(4) 0.020(3) 0.004(3) 0.002(3) -0.024(4) C4 0.034(4) 0.041(4) 0.027(3) -0.006(3) 0.011(3) -0.025(4) C5 0.032(4) 0.049(5) 0.036(4) -0.003(3) 0.002(3) -0.025(4) C6 0.025(3) 0.042(4) 0.031(3) 0.011(3) -0.004(3) -0.017(3) C7 0.025(3) 0.024(3) 0.021(3) 0.005(2) -0.003(2) -0.011(3) C8 0.024(3) 0.030(3) 0.022(3) 0.000(2) 0.004(2) -0.016(3) C9 0.023(3) 0.023(3) 0.019(3) -0.002(2) -0.003(2) -0.008(2) C10 0.022(3) 0.034(4) 0.028(3) -0.001(3) -0.001(2) -0.011(3) C11 0.020(3) 0.023(3) 0.027(3) 0.004(2) -0.004(2) -0.007(3) C12 0.028(3) 0.022(3) 0.032(3) -0.005(2) -0.004(3) -0.008(3) C13 0.033(4) 0.028(3) 0.030(3) 0.000(3) 0.000(3) -0.019(3) C14 0.033(4) 0.019(3) 0.029(3) -0.003(2) -0.003(3) -0.011(3) C15 0.033(4) 0.033(4) 0.030(3) -0.003(3) -0.003(3) -0.018(3) C16 0.033(4) 0.034(4) 0.028(3) 0.002(3) -0.001(3) -0.020(3) C17 0.030(3) 0.037(4) 0.017(3) 0.002(2) -0.006(2) -0.021(3) C18 0.032(4) 0.031(3) 0.024(3) 0.002(2) -0.002(2) -0.020(3) C19 0.046(4) 0.043(4) 0.022(3) 0.011(3) -0.007(3) -0.030(4) C20 0.032(4) 0.036(4) 0.025(3) -0.003(3) 0.002(3) -0.022(3) C21 0.038(4) 0.063(6) 0.039(4) 0.012(4) -0.011(3) -0.032(4) C22 0.035(4) 0.060(5) 0.035(4) 0.021(4) -0.014(3) -0.030(4) C23 0.027(3) 0.027(3) 0.020(3) 0.007(2) -0.007(2) -0.014(3) C24 0.023(3) 0.032(3) 0.020(3) 0.000(2) 0.005(2) -0.017(3) C25 0.023(3) 0.027(3) 0.020(3) 0.000(2) -0.003(2) -0.011(3) C26 0.025(3) 0.028(4) 0.033(3) 0.003(3) -0.001(3) -0.011(3) C27 0.025(3) 0.029(4) 0.021(3) 0.003(2) -0.004(2) -0.011(3) C28 0.027(3) 0.028(4) 0.031(3) -0.005(3) -0.005(3) -0.011(3) C29 0.034(4) 0.022(3) 0.029(3) -0.003(2) 0.001(3) -0.016(3) C30 0.031(4) 0.026(3) 0.028(3) -0.005(2) -0.003(3) -0.018(3) C31 0.037(4) 0.032(4) 0.029(3) 0.002(3) -0.009(3) -0.017(3) C32 0.041(4) 0.043(4) 0.026(3) 0.002(3) -0.003(3) -0.029(3) C33 0.030(4) 0.033(4) 0.023(3) 0.004(3) -0.006(3) -0.022(3) C34 0.039(4) 0.035(4) 0.024(3) 0.005(3) -0.006(3) -0.020(3) C35 0.049(5) 0.050(5) 0.022(3) 0.010(3) -0.005(3) -0.034(4) C36 0.044(5) 0.042(4) 0.028(3) -0.002(3) 0.001(3) -0.029(4) C37 0.028(4) 0.046(5) 0.040(4) 0.006(3) -0.002(3) -0.017(4) C38 0.032(4) 0.053(5) 0.033(4) 0.006(3) -0.011(3) -0.022(4) C39 0.025(3) 0.030(3) 0.019(3) 0.005(2) -0.003(2) -0.017(3) C40 0.038(4) 0.040(4) 0.024(3) -0.002(3) -0.002(3) -0.026(3) C41 0.033(4) 0.037(4) 0.023(3) 0.000(3) -0.008(3) -0.018(3) C42 0.036(4) 0.030(4) 0.025(3) 0.003(3) 0.000(3) -0.017(3) C43 0.030(4) 0.030(4) 0.025(3) 0.004(3) -0.002(3) -0.010(3) C44 0.029(4) 0.038(4) 0.031(3) -0.011(3) 0.007(3) -0.021(3) C45 0.037(4) 0.031(4) 0.030(3) -0.006(3) 0.004(3) -0.018(3) C46 0.029(3) 0.035(4) 0.030(3) -0.011(3) 0.003(3) -0.020(3) C47 0.033(4) 0.043(4) 0.031(3) -0.003(3) -0.005(3) -0.024(3) C48 0.044(4) 0.048(5) 0.031(3) -0.003(3) -0.006(3) -0.030(4) C49 0.025(3) 0.023(3) 0.025(3) 0.003(2) -0.005(2) -0.013(3) C50 0.039(4) 0.026(3) 0.021(3) 0.002(2) -0.003(3) -0.014(3) C51 0.045(4) 0.050(5) 0.023(3) 0.007(3) -0.003(3) -0.026(4) C52 0.036(4) 0.040(4) 0.026(3) 0.000(3) 0.003(3) -0.026(3) C53 0.036(4) 0.063(6) 0.043(4) 0.012(4) -0.005(3) -0.032(4) C54 0.032(4) 0.055(5) 0.037(4) 0.017(4) -0.012(3) -0.021(4) C55 0.026(3) 0.025(3) 0.021(3) 0.001(2) 0.005(2) -0.016(3) C56 0.037(4) 0.027(4) 0.029(3) 0.000(3) -0.005(3) -0.019(3) C57 0.030(3) 0.028(3) 0.025(3) 0.000(2) -0.007(3) -0.013(3) C58 0.031(4) 0.036(4) 0.026(3) 0.000(3) -0.003(3) -0.016(3) C59 0.025(3) 0.026(3) 0.030(3) 0.006(3) -0.005(3) -0.008(3) C60 0.030(4) 0.034(4) 0.032(3) -0.008(3) 0.002(3) -0.020(3) C61 0.030(4) 0.037(4) 0.031(3) -0.003(3) 0.002(3) -0.020(3) C62 0.032(4) 0.031(4) 0.026(3) -0.006(3) 0.000(3) -0.017(3) C63 0.039(4) 0.046(4) 0.026(3) -0.004(3) -0.003(3) -0.029(4) C64 0.037(4) 0.048(5) 0.030(3) -0.002(3) -0.003(3) -0.027(4) N1 0.031(3) 0.034(3) 0.018(2) 0.004(2) -0.001(2) -0.018(3) N2 0.025(3) 0.025(3) 0.018(2) 0.0021(19) 0.001(2) -0.014(2) N3 0.033(3) 0.028(3) 0.020(2) 0.002(2) -0.002(2) -0.018(3) N4 0.023(3) 0.026(3) 0.018(2) 0.0027(19) 0.000(2) -0.011(2) N5 0.025(3) 0.031(3) 0.018(2) -0.001(2) -0.001(2) -0.016(2) N6 0.044(4) 0.032(3) 0.019(3) 0.002(2) -0.006(2) -0.023(3) N7 0.027(3) 0.028(3) 0.023(2) 0.001(2) -0.002(2) -0.016(2) N8 0.042(3) 0.030(3) 0.021(3) 0.001(2) -0.005(2) -0.020(3) O1 0.023(2) 0.023(2) 0.028(2) 0.0041(17) -0.0043(17) -0.0126(19) O2 0.029(2) 0.030(3) 0.026(2) 0.0043(18) -0.0076(18) -0.018(2) O3 0.029(2) 0.028(3) 0.027(2) 0.0034(18) -0.0056(18) -0.012(2) O4 0.028(2) 0.026(2) 0.027(2) 0.0037(17) -0.0054(18) -0.014(2) O5 0.024(2) 0.030(2) 0.031(2) 0.0028(17) -0.0060(17) -0.0157(19) O6 0.026(3) 0.031(3) 0.115(6) 0.002(3) -0.007(3) -0.010(2) O7 0.045(3) 0.035(3) 0.030(2) 0.0093(18) -0.0069(19) -0.021(2) O9 0.028(2) 0.028(2) 0.031(2) 0.0069(17) -0.0072(18) -0.0158(19) O13 0.123(8) 0.064(5) 0.085(6) 0.025(4) -0.077(6) -0.050(5) O14 0.025(2) 0.030(2) 0.037(2) -0.0002(18) -0.0023(18) -0.0127(19) O15 0.026(2) 0.031(3) 0.046(3) -0.004(2) -0.002(2) -0.014(2) O16 0.030(2) 0.028(2) 0.035(2) -0.0015(18) -0.0020(19) -0.014(2) O17 0.029(2) 0.031(2) 0.028(2) 0.0068(17) -0.0059(18) -0.018(2) O18 0.034(3) 0.035(3) 0.029(2) -0.0018(18) -0.0022(19) -0.019(2) O19 0.041(3) 0.040(3) 0.026(2) 0.002(2) -0.007(2) -0.020(2) O20 0.021(2) 0.024(2) 0.039(2) 0.0014(18) -0.0078(18) -0.0098(18) O21 0.018(2) 0.026(2) 0.043(3) -0.0015(19) -0.0077(18) -0.0064(18) O22 0.075(5) 0.048(4) 0.040(3) 0.010(3) -0.028(3) -0.029(3) O23 0.041(3) 0.055(3) 0.032(2) -0.004(2) 0.000(2) -0.032(3) O24 0.037(3) 0.059(3) 0.029(2) 0.000(2) -0.002(2) -0.030(3) O25 0.048(3) 0.039(3) 0.027(2) 0.000(2) -0.005(2) -0.024(3) O26 0.028(2) 0.030(2) 0.026(2) 0.0060(17) -0.0047(17) -0.018(2) S1 0.0277(8) 0.0371(10) 0.0358(9) 0.0047(7) -0.0023(7) -0.0193(8) S2 0.0293(8) 0.0365(9) 0.0317(9) -0.0004(7) -0.0010(7) -0.0197(7) S3 0.0338(9) 0.0412(10) 0.0339(9) -0.0017(7) 0.0020(7) -0.0236(8) S4 0.0311(9) 0.0447(11) 0.0354(9) -0.0031(7) 0.0014(7) -0.0230(8) S5 0.0194(6) 0.0223(6) 0.0282(7) 0.0056(5) -0.0045(5) -0.0097(5) S6 0.0202(6) 0.0247(7) 0.0308(8) 0.0097(5) -0.0052(5) -0.0105(5) Cl1A 0.0372(12) 0.051(2) 0.0308(14) 0.0170(13) -0.0153(8) -0.0252(11) Cl2 0.0525(12) 0.0631(14) 0.0289(8) -0.0050(8) 0.0115(8) -0.0416(11) Cl3 0.0346(9) 0.0392(10) 0.0352(9) 0.0094(7) -0.0029(7) -0.0165(8) Cl4 0.0341(10) 0.0506(13) 0.0501(12) 0.0297(10) -0.0072(8) -0.0116(9) Cl5A 0.0381(17) 0.053(2) 0.0270(10) 0.0043(9) 0.0061(8) -0.0297(18) Cl6 0.0328(8) 0.0323(9) 0.0301(8) 0.0043(6) -0.0020(6) -0.0132(7) Cl7 0.0417(10) 0.0623(14) 0.0395(10) 0.0251(9) -0.0157(8) -0.0273(10) Cl8 0.0588(14) 0.0746(17) 0.0322(9) -0.0035(9) 0.0101(9) -0.0501(13) Cl9 0.0417(10) 0.0407(10) 0.0343(9) 0.0034(7) 0.0011(7) -0.0205(8) Cl1C 0.0299(12) 0.036(2) 0.0462(18) 0.0208(15) -0.0066(9) -0.0100(10) Cl11 0.0460(11) 0.0592(13) 0.0327(9) -0.0003(8) 0.0069(8) -0.0348(10) Cl12 0.0363(9) 0.0385(10) 0.0374(9) 0.0061(7) -0.0011(7) -0.0165(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' 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' S S 0.3331 0.5567 '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' 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 C6 C1 C2 117.0(6) . . ? C6 C1 C7 120.2(6) . . ? C2 C1 C7 122.8(7) . . ? C1 C2 C3 122.5(7) . . ? C1 C2 Cl1B 117.9(8) . . ? C3 C2 Cl1B 116.8(8) . . ? C1 C2 Cl1A 120.5(6) . . ? C3 C2 Cl1A 116.9(6) . . ? Cl1B C2 Cl1A 20.4(9) . . ? C4 C3 C2 117.5(7) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 122.1(6) . . ? C5 C4 Cl2 118.7(6) . . ? C3 C4 Cl2 119.2(6) . . ? C4 C5 C6 118.5(8) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C1 C6 C5 122.3(7) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? O1 C7 C1 111.4(5) . . ? O1 C7 C8 107.2(5) . . ? C1 C7 C8 109.6(6) . . ? O1 C7 H7 109.5 . . ? C1 C7 H7 109.5 . . ? C8 C7 H7 109.5 . . ? N2 C8 C7 110.9(6) . . ? N2 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.0 . . ? N2 C9 N1 108.5(6) . . ? N2 C9 H9 125.7 . . ? N1 C9 H9 125.7 . . ? C11 C10 N1 107.1(6) . . ? C11 C10 H10 126.4 . . ? N1 C10 H10 126.4 . . ? C10 C11 N2 106.9(6) . . ? C10 C11 H11 126.6 . . ? N2 C11 H11 126.6 . . ? O1 C12 C14 111.7(5) . . ? O1 C12 H12A 109.3 . . ? C14 C12 H12A 109.3 . . ? O1 C12 H12B 109.3 . . ? C14 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C14 C13 Cl3 127.4(6) . . ? C14 C13 S1 112.8(5) . . ? Cl3 C13 S1 119.8(5) . . ? C13 C14 C15 110.2(7) . . ? C13 C14 C12 126.9(6) . . ? C15 C14 C12 122.9(7) . . ? C16 C15 C14 114.5(7) . . ? C16 C15 H15 122.8 . . ? C14 C15 H15 122.8 . . ? C15 C16 S1 111.5(6) . . ? C15 C16 H16 124.3 . . ? S1 C16 H16 124.3 . . ? C18 C17 C22 117.9(6) . . ? C18 C17 C23 122.5(6) . . ? C22 C17 C23 119.6(6) . . ? C17 C18 C19 121.5(7) . . ? C17 C18 Cl4 120.3(5) . . ? C19 C18 Cl4 118.3(6) . . ? C20 C19 C18 118.5(7) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C19 C20 C21 121.6(7) . . ? C19 C20 Cl5A 120.4(6) . . ? C21 C20 Cl5A 118.0(6) . . ? C19 C20 Cl5B 103.4(14) . . ? C21 C20 Cl5B 133.4(13) . . ? Cl5A C20 Cl5B 20.6(13) . . ? C22 C21 C20 118.7(8) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C17 121.8(7) . . ? C21 C22 H22 119.1 . . ? C17 C22 H22 119.1 . . ? O2 C23 C17 112.3(6) . . ? O2 C23 C24 107.4(5) . . ? C17 C23 C24 109.3(5) . . ? O2 C23 H23 109.3 . . ? C17 C23 H23 109.3 . . ? C24 C23 H23 109.3 . . ? N4 C24 C23 110.4(5) . . ? N4 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N4 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? N4 C25 N3 108.5(6) . . ? N4 C25 H25 125.8 . . ? N3 C25 H25 125.8 . . ? C27 C26 N3 107.0(6) . . ? C27 C26 H26 126.5 . . ? N3 C26 H26 126.5 . . ? C26 C27 N4 107.0(6) . . ? C26 C27 H27 126.5 . . ? N4 C27 H27 126.5 . . ? O2 C28 C30 110.7(5) . . ? O2 C28 H28A 109.5 . . ? C30 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? C30 C28 H28B 109.5 . . ? H28A C28 H28B 108.1 . . ? C30 C29 Cl6 127.1(6) . . ? C30 C29 S2 113.0(5) . . ? Cl6 C29 S2 119.9(5) . . ? C29 C30 C31 110.6(6) . . ? C29 C30 C28 126.2(6) . . ? C31 C30 C28 123.2(7) . . ? C32 C31 C30 113.1(7) . . ? C32 C31 H31 123.4 . . ? C30 C31 H31 123.4 . . ? C31 C32 S2 112.5(5) . . ? C31 C32 H32 123.8 . . ? S2 C32 H32 123.8 . . ? C34 C33 C38 117.0(7) . . ? C34 C33 C39 123.7(7) . . ? C38 C33 C39 119.3(6) . . ? C33 C34 C35 123.1(8) . . ? C33 C34 Cl7 121.1(6) . . ? C35 C34 Cl7 115.8(6) . . ? C36 C35 C34 118.5(7) . . ? C36 C35 H35 120.8 . . ? C34 C35 H35 120.8 . . ? C35 C36 C37 120.0(7) . . ? C35 C36 Cl8 120.3(6) . . ? C37 C36 Cl8 119.6(7) . . ? C38 C37 C36 120.0(8) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 121.3(7) . . ? C37 C38 H38 119.3 . . ? C33 C38 H38 119.3 . . ? O3 C39 C33 111.0(5) . . ? O3 C39 C40 107.2(5) . . ? C33 C39 C40 110.2(6) . . ? O3 C39 H39 109.5 . . ? C33 C39 H39 109.5 . . ? C40 C39 H39 109.5 . . ? N5 C40 C39 110.2(6) . . ? N5 C40 H40A 109.6 . . ? C39 C40 H40A 109.6 . . ? N5 C40 H40B 109.6 . . ? C39 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? N6 C41 N5 108.5(7) . . ? N6 C41 H41 125.8 . . ? N5 C41 H41 125.8 . . ? C43 C42 N6 106.1(7) . . ? C43 C42 H42 126.9 . . ? N6 C42 H42 126.9 . . ? C42 C43 N5 107.1(6) . . ? C42 C43 H43 126.5 . . ? N5 C43 H43 126.5 . . ? O3 C44 C46 110.5(5) . . ? O3 C44 H44A 109.6 . . ? C46 C44 H44A 109.6 . . ? O3 C44 H44B 109.6 . . ? C46 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? C46 C45 S3 113.5(6) . . ? C46 C45 Cl9 128.1(6) . . ? S3 C45 Cl9 118.3(5) . . ? C45 C46 C47 110.9(7) . . ? C45 C46 C44 126.9(7) . . ? C47 C46 C44 122.1(7) . . ? C48 C47 C46 113.3(7) . . ? C48 C47 H47 123.3 . . ? C46 C47 H47 123.3 . . ? C47 C48 S3 111.4(6) . . ? C47 C48 H48 124.3 . . ? S3 C48 H48 124.3 . . ? C54 C49 C50 117.5(7) . . ? C54 C49 C55 121.1(6) . . ? C50 C49 C55 121.4(6) . . ? C49 C50 C51 122.5(8) . . ? C49 C50 Cl1C 121.1(6) . . ? C51 C50 Cl1C 116.3(6) . . ? C49 C50 Cl1D 119.4(8) . . ? C51 C50 Cl1D 115.1(8) . . ? Cl1C C50 Cl1D 20.2(8) . . ? C52 C51 C50 117.7(7) . . ? C52 C51 H51 121.2 . . ? C50 C51 H51 121.2 . . ? C53 C52 C51 121.0(7) . . ? C53 C52 Cl11 120.0(7) . . ? C51 C52 Cl11 119.1(6) . . ? C52 C53 C54 119.6(8) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C49 C54 C53 121.8(8) . . ? C49 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? O4 C55 C56 107.7(5) . . ? O4 C55 C49 110.3(5) . . ? C56 C55 C49 109.6(6) . . ? O4 C55 H55 109.7 . . ? C56 C55 H55 109.7 . . ? C49 C55 H55 109.7 . . ? N7 C56 C55 110.5(6) . . ? N7 C56 H56A 109.6 . . ? C55 C56 H56A 109.6 . . ? N7 C56 H56B 109.6 . . ? C55 C56 H56B 109.6 . . ? H56A C56 H56B 108.1 . . ? N8 C57 N7 109.1(6) . . ? N8 C57 H57 125.4 . . ? N7 C57 H57 125.4 . . ? C59 C58 N8 106.7(7) . . ? C59 C58 H58 126.6 . . ? N8 C58 H58 126.6 . . ? C58 C59 N7 107.0(6) . . ? C58 C59 H59 126.5 . . ? N7 C59 H59 126.5 . . ? O4 C60 C62 110.5(6) . . ? O4 C60 H60A 109.6 . . ? C62 C60 H60A 109.6 . . ? O4 C60 H60B 109.6 . . ? C62 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? C62 C61 S4 114.4(6) . . ? C62 C61 Cl12 127.3(6) . . ? S4 C61 Cl12 118.3(5) . . ? C61 C62 C63 110.3(7) . . ? C61 C62 C60 126.8(7) . . ? C63 C62 C60 122.9(7) . . ? C64 C63 C62 112.8(7) . . ? C64 C63 H63 123.6 . . ? C62 C63 H63 123.6 . . ? C63 C64 S4 112.3(6) . . ? C63 C64 H64 123.9 . . ? S4 C64 H64 123.9 . . ? C9 N1 C10 109.0(6) . . ? C9 N1 H1N 125.5 . . ? C10 N1 H1N 125.5 . . ? C9 N2 C11 108.5(5) . . ? C9 N2 C8 126.2(6) . . ? C11 N2 C8 125.3(6) . . ? C25 N3 C26 108.8(6) . . ? C25 N3 H3N 125.6 . . ? C26 N3 H3N 125.6 . . ? C25 N4 C27 108.8(5) . . ? C25 N4 C24 125.6(6) . . ? C27 N4 C24 125.4(6) . . ? C41 N5 C43 108.0(6) . . ? C41 N5 C40 127.5(6) . . ? C43 N5 C40 124.5(6) . . ? C41 N6 C42 110.3(6) . . ? C41 N6 H6N 131(9) . . ? C42 N6 H6N 117(9) . . ? C57 N7 C59 107.6(6) . . ? C57 N7 C56 127.2(6) . . ? C59 N7 C56 125.2(6) . . ? C57 N8 C58 109.6(6) . . ? C57 N8 H8N 128(8) . . ? C58 N8 H8N 122(8) . . ? C12 O1 C7 113.5(5) . . ? C23 O2 C28 113.2(5) . . ? C39 O3 C44 113.0(5) . . ? C55 O4 C60 113.1(5) . . ? O10B O10A S6 69.9(10) . . ? O10A O10B S6 76.7(10) . . ? O10A O10B O11A 126.6(12) . . ? S6 O10B O11A 50.6(5) . . ? O11B O11A S6 87.0(15) . . ? O11B O11A O10B 136.2(16) . . ? S6 O11A O10B 50.7(5) . . ? O11A O11B S6 66.1(13) . . ? O12B O12A S6 79(2) . . ? O12A O12B S6 81(2) . . ? H13A O13 H13B 87(4) . . ? H14A O14 H14B 85(4) . . ? H15A O15 H15B 87(4) . . ? H16A O16 H16B 85(4) . . ? H17A O17 H17B 86(4) . . ? H18A O18 H18B 86(9) . . ? H19A O19 H19B 85(4) . . ? H20A O20 H20B 83(4) . . ? H21A O21 H21B 85(4) . . ? H22A O22 H22B 88(4) . . ? H23A O23 H23B 91(4) . . ? H24C O24 H24D 85(4) . . ? H25A O25 H25B 83(4) . . ? H26A O26 H26B 83(4) . . ? C16 S1 C13 91.0(4) . . ? C32 S2 C29 90.7(4) . . ? C45 S3 C48 90.8(4) . . ? C61 S4 C64 90.2(4) . . ? O8A S5 O7 114.0(8) . . ? O8A S5 O6 103.0(10) . . ? O7 S5 O6 109.8(4) . . ? O8A S5 O5 109.4(4) . . ? O7 S5 O5 111.0(3) . . ? O6 S5 O5 109.4(3) . . ? O8A S5 O8B 14.4(8) . . ? O7 S5 O8B 103.4(11) . . ? O6 S5 O8B 116.7(14) . . ? O5 S5 O8B 106.5(6) . . ? O11A S6 O10B 78.7(6) . . ? O11A S6 O12B 125.9(7) . . ? O10B S6 O12B 110.7(7) . . ? O11A S6 O10A 111.7(7) . . ? O10B S6 O10A 33.4(5) . . ? O12B S6 O10A 86.7(8) . . ? O11A S6 O12A 113.3(7) . . ? O10B S6 O12A 126.7(5) . . ? O12B S6 O12A 19.9(5) . . ? O10A S6 O12A 106.2(6) . . ? O11A S6 O9 112.5(5) . . ? O10B S6 O9 114.1(4) . . ? O12B S6 O9 110.8(5) . . ? O10A S6 O9 104.3(5) . . ? O12A S6 O9 108.2(4) . . ? O11A S6 O11B 27.0(5) . . ? O10B S6 O11B 105.1(5) . . ? O12B S6 O11B 110.0(7) . . ? O10A S6 O11B 137.0(6) . . ? O12A S6 O11B 92.6(5) . . ? O9 S6 O11B 105.8(4) . . ? Cl1B Cl1A C2 67.8(16) . . ? Cl1A Cl1B C2 91.7(16) . . ? Cl5B Cl5A C20 86(2) . . ? Cl5A Cl5B C20 74(2) . . ? Cl1D Cl1C C50 87.9(18) . . ? Cl1C Cl1D C50 71.9(17) . . ? 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 C1 C6 1.384(11) . ? C1 C2 1.386(10) . ? C1 C7 1.511(9) . ? C2 C3 1.395(10) . ? C2 Cl1B 1.628(18) . ? C2 Cl1A 1.757(8) . ? C3 C4 1.384(12) . ? C3 H3 0.9500 . ? C4 C5 1.369(12) . ? C4 Cl2 1.731(7) . ? C5 C6 1.388(10) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.435(8) . ? C7 C8 1.517(9) . ? C7 H7 1.0000 . ? C8 N2 1.456(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.334(8) . ? C9 N1 1.336(9) . ? C9 H9 0.9500 . ? C10 C11 1.364(10) . ? C10 N1 1.368(10) . ? C10 H10 0.9500 . ? C11 N2 1.382(9) . ? C11 H11 0.9500 . ? C12 O1 1.428(8) . ? C12 C14 1.507(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.355(11) . ? C13 Cl3 1.703(7) . ? C13 S1 1.729(7) . ? C14 C15 1.434(10) . ? C15 C16 1.338(11) . ? C15 H15 0.9500 . ? C16 S1 1.717(8) . ? C16 H16 0.9500 . ? C17 C18 1.380(10) . ? C17 C22 1.401(11) . ? C17 C23 1.510(9) . ? C18 C19 1.404(10) . ? C18 Cl4 1.713(8) . ? C19 C20 1.378(12) . ? C19 H19 0.9500 . ? C20 C21 1.385(12) . ? C20 Cl5A 1.736(7) . ? C20 Cl5B 1.80(3) . ? C21 C22 1.379(11) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O2 1.430(8) . ? C23 C24 1.533(9) . ? C23 H23 1.0000 . ? C24 N4 1.460(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 N4 1.328(8) . ? C25 N3 1.343(9) . ? C25 H25 0.9500 . ? C26 C27 1.363(10) . ? C26 N3 1.374(10) . ? C26 H26 0.9500 . ? C27 N4 1.382(9) . ? C27 H27 0.9500 . ? C28 O2 1.434(9) . ? C28 C30 1.512(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.360(11) . ? C29 Cl6 1.702(7) . ? C29 S2 1.729(7) . ? C30 C31 1.432(10) . ? C31 C32 1.358(11) . ? C31 H31 0.9500 . ? C32 S2 1.704(8) . ? C32 H32 0.9500 . ? C33 C34 1.375(10) . ? C33 C38 1.388(11) . ? C33 C39 1.520(9) . ? C34 C35 1.391(10) . ? C34 Cl7 1.758(8) . ? C35 C36 1.371(13) . ? C35 H35 0.9500 . ? C36 C37 1.388(12) . ? C36 Cl8 1.735(8) . ? C37 C38 1.380(11) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 O3 1.419(8) . ? C39 C40 1.526(9) . ? C39 H39 1.0000 . ? C40 N5 1.462(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 N6 1.306(10) . ? C41 N5 1.335(9) . ? C41 H41 0.9500 . ? C42 C43 1.352(10) . ? C42 N6 1.375(10) . ? C42 H42 0.9500 . ? C43 N5 1.392(9) . ? C43 H43 0.9500 . ? C44 O3 1.441(9) . ? C44 C46 1.511(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.360(12) . ? C45 S3 1.717(8) . ? C45 Cl9 1.741(8) . ? C46 C47 1.427(11) . ? C47 C48 1.365(11) . ? C47 H47 0.9500 . ? C48 S3 1.730(9) . ? C48 H48 0.9500 . ? C49 C54 1.365(11) . ? C49 C50 1.391(9) . ? C49 C55 1.526(8) . ? C50 C51 1.393(10) . ? C50 Cl1C 1.753(8) . ? C50 Cl1D 1.84(2) . ? C51 C52 1.388(12) . ? C51 H51 0.9500 . ? C52 C53 1.367(12) . ? C52 Cl11 1.741(7) . ? C53 C54 1.391(11) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 O4 1.426(8) . ? C55 C56 1.521(9) . ? C55 H55 1.0000 . ? C56 N7 1.465(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 N8 1.309(10) . ? C57 N7 1.334(9) . ? C57 H57 0.9500 . ? C58 C59 1.353(10) . ? C58 N8 1.366(10) . ? C58 H58 0.9500 . ? C59 N7 1.388(9) . ? C59 H59 0.9500 . ? C60 O4 1.444(9) . ? C60 C62 1.489(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.368(11) . ? C61 S4 1.715(7) . ? C61 Cl12 1.739(8) . ? C62 C63 1.439(10) . ? C63 C64 1.370(11) . ? C63 H63 0.9500 . ? C64 S4 1.734(9) . ? C64 H64 0.9500 . ? N1 H1N 0.8800 . ? N3 H3N 0.8800 . ? N6 H6N 0.77(13) . ? N8 H8N 0.79(12) . ? O5 S5 1.497(5) . ? O6 S5 1.464(6) . ? O7 S5 1.448(5) . ? O8A S5 1.419(10) . ? O8B S5 1.56(2) . ? O9 S6 1.497(5) . ? O10A O10B 0.833(13) . ? O10A S6 1.475(12) . ? O10B S6 1.424(8) . ? O10B O11A 1.805(15) . ? O11A O11B 0.705(13) . ? O11A S6 1.422(12) . ? O11B S6 1.553(10) . ? O12A O12B 0.508(13) . ? O12A S6 1.479(9) . ? O12B S6 1.466(12) . ? O13 H13A 0.96(2) . ? O13 H13B 0.89(2) . ? O14 H14A 0.96(2) . ? O14 H14B 0.90(2) . ? O15 H15A 0.97(2) . ? O15 H15B 0.88(2) . ? O16 H16A 0.97(2) . ? O16 H16B 0.90(2) . ? O17 H17A 0.97(2) . ? O17 H17B 0.90(2) . ? O18 H18A 0.99(13) . ? O18 H18B 0.89(9) . ? O19 H19A 0.96(2) . ? O19 H19B 0.90(2) . ? O20 H20A 0.96(2) . ? O20 H20B 0.90(2) . ? O21 H21A 0.96(2) . ? O21 H21B 0.88(2) . ? O22 H22A 0.96(2) . ? O22 H22B 0.89(2) . ? O23 H23A 0.95(2) . ? O23 H23B 0.89(2) . ? O24 H24C 0.97(2) . ? O24 H24D 0.90(2) . ? O25 H25A 0.97(2) . ? O25 H25B 0.90(2) . ? O26 H26A 0.97(2) . ? O26 H26B 0.90(2) . ? Cl1A Cl1B 0.61(3) . ? Cl5A Cl5B 0.63(4) . ? Cl1C Cl1D 0.64(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.3(11) . . . . ? C7 C1 C2 C3 179.7(7) . . . . ? C6 C1 C2 Cl1B -159.1(13) . . . . ? C7 C1 C2 Cl1B 19.2(15) . . . . ? C6 C1 C2 Cl1A 177.6(6) . . . . ? C7 C1 C2 Cl1A -4.0(10) . . . . ? C1 C2 C3 C4 -0.6(12) . . . . ? Cl1B C2 C3 C4 160.0(13) . . . . ? Cl1A C2 C3 C4 -177.1(6) . . . . ? C2 C3 C4 C5 -1.0(12) . . . . ? C2 C3 C4 Cl2 179.8(6) . . . . ? C3 C4 C5 C6 1.8(12) . . . . ? Cl2 C4 C5 C6 -179.0(6) . . . . ? C2 C1 C6 C5 -0.4(12) . . . . ? C7 C1 C6 C5 -178.8(7) . . . . ? C4 C5 C6 C1 -1.1(13) . . . . ? C6 C1 C7 O1 -57.5(9) . . . . ? C2 C1 C7 O1 124.2(7) . . . . ? C6 C1 C7 C8 61.0(9) . . . . ? C2 C1 C7 C8 -117.3(7) . . . . ? O1 C7 C8 N2 -67.5(7) . . . . ? C1 C7 C8 N2 171.4(5) . . . . ? N1 C10 C11 N2 0.0(8) . . . . ? Cl3 C13 C14 C15 -177.8(6) . . . . ? S1 C13 C14 C15 0.4(7) . . . . ? Cl3 C13 C14 C12 3.9(11) . . . . ? S1 C13 C14 C12 -178.0(5) . . . . ? O1 C12 C14 C13 118.2(7) . . . . ? O1 C12 C14 C15 -60.0(9) . . . . ? C13 C14 C15 C16 -0.3(9) . . . . ? C12 C14 C15 C16 178.2(6) . . . . ? C14 C15 C16 S1 0.1(8) . . . . ? C22 C17 C18 C19 0.7(11) . . . . ? C23 C17 C18 C19 179.3(7) . . . . ? C22 C17 C18 Cl4 -177.1(6) . . . . ? C23 C17 C18 Cl4 1.6(10) . . . . ? C17 C18 C19 C20 0.4(11) . . . . ? Cl4 C18 C19 C20 178.2(6) . . . . ? C18 C19 C20 C21 -1.6(12) . . . . ? C18 C19 C20 Cl5A 178.9(6) . . . . ? C18 C19 C20 Cl5B -168.7(12) . . . . ? C19 C20 C21 C22 1.6(13) . . . . ? Cl5A C20 C21 C22 -178.8(7) . . . . ? Cl5B C20 C21 C22 164.2(18) . . . . ? C20 C21 C22 C17 -0.4(14) . . . . ? C18 C17 C22 C21 -0.7(13) . . . . ? C23 C17 C22 C21 -179.3(8) . . . . ? C18 C17 C23 O2 136.9(7) . . . . ? C22 C17 C23 O2 -44.5(9) . . . . ? C18 C17 C23 C24 -104.0(7) . . . . ? C22 C17 C23 C24 74.6(9) . . . . ? O2 C23 C24 N4 -66.6(7) . . . . ? C17 C23 C24 N4 171.4(5) . . . . ? N3 C26 C27 N4 -0.9(8) . . . . ? Cl6 C29 C30 C31 -178.4(5) . . . . ? S2 C29 C30 C31 1.1(7) . . . . ? Cl6 C29 C30 C28 2.4(10) . . . . ? S2 C29 C30 C28 -178.1(5) . . . . ? O2 C28 C30 C29 110.3(7) . . . . ? O2 C28 C30 C31 -68.8(9) . . . . ? C29 C30 C31 C32 -0.9(9) . . . . ? C28 C30 C31 C32 178.4(7) . . . . ? C30 C31 C32 S2 0.3(8) . . . . ? C38 C33 C34 C35 -1.3(12) . . . . ? C39 C33 C34 C35 -179.8(7) . . . . ? C38 C33 C34 Cl7 177.9(6) . . . . ? C39 C33 C34 Cl7 -0.6(10) . . . . ? C33 C34 C35 C36 -1.5(13) . . . . ? Cl7 C34 C35 C36 179.2(6) . . . . ? C34 C35 C36 C37 3.4(13) . . . . ? C34 C35 C36 Cl8 -178.6(6) . . . . ? C35 C36 C37 C38 -2.4(13) . . . . ? Cl8 C36 C37 C38 179.5(7) . . . . ? C36 C37 C38 C33 -0.5(14) . . . . ? C34 C33 C38 C37 2.3(12) . . . . ? C39 C33 C38 C37 -179.1(8) . . . . ? C34 C33 C39 O3 -122.1(7) . . . . ? C38 C33 C39 O3 59.4(9) . . . . ? C34 C33 C39 C40 119.2(8) . . . . ? C38 C33 C39 C40 -59.2(9) . . . . ? O3 C39 C40 N5 69.9(7) . . . . ? C33 C39 C40 N5 -169.1(6) . . . . ? N6 C42 C43 N5 0.4(8) . . . . ? S3 C45 C46 C47 -1.7(8) . . . . ? Cl9 C45 C46 C47 178.6(6) . . . . ? S3 C45 C46 C44 176.9(6) . . . . ? Cl9 C45 C46 C44 -2.8(11) . . . . ? O3 C44 C46 C45 -119.1(8) . . . . ? O3 C44 C46 C47 59.3(9) . . . . ? C45 C46 C47 C48 1.9(9) . . . . ? C44 C46 C47 C48 -176.8(7) . . . . ? C46 C47 C48 S3 -1.2(9) . . . . ? C54 C49 C50 C51 -2.6(11) . . . . ? C55 C49 C50 C51 179.7(7) . . . . ? C54 C49 C50 Cl1C 174.7(7) . . . . ? C55 C49 C50 Cl1C -3.0(10) . . . . ? C54 C49 C50 Cl1D -161.9(13) . . . . ? C55 C49 C50 Cl1D 20.4(14) . . . . ? C49 C50 C51 C52 1.4(12) . . . . ? Cl1C C50 C51 C52 -176.1(6) . . . . ? Cl1D C50 C51 C52 161.5(13) . . . . ? C50 C51 C52 C53 0.6(12) . . . . ? C50 C51 C52 Cl11 -179.4(6) . . . . ? C51 C52 C53 C54 -1.3(14) . . . . ? Cl11 C52 C53 C54 178.8(7) . . . . ? C50 C49 C54 C53 1.9(13) . . . . ? C55 C49 C54 C53 179.6(8) . . . . ? C52 C53 C54 C49 0.0(15) . . . . ? C54 C49 C55 O4 44.1(9) . . . . ? C50 C49 C55 O4 -138.3(7) . . . . ? C54 C49 C55 C56 -74.4(9) . . . . ? C50 C49 C55 C56 103.2(8) . . . . ? O4 C55 C56 N7 68.8(7) . . . . ? C49 C55 C56 N7 -171.2(6) . . . . ? N8 C58 C59 N7 -1.0(8) . . . . ? S4 C61 C62 C63 -0.8(8) . . . . ? Cl12 C61 C62 C63 179.2(6) . . . . ? S4 C61 C62 C60 176.6(6) . . . . ? Cl12 C61 C62 C60 -3.5(11) . . . . ? O4 C60 C62 C61 -108.6(8) . . . . ? O4 C60 C62 C63 68.4(9) . . . . ? C61 C62 C63 C64 1.4(9) . . . . ? C60 C62 C63 C64 -176.1(7) . . . . ? C62 C63 C64 S4 -1.4(9) . . . . ? N2 C9 N1 C10 0.1(8) . . . . ? C11 C10 N1 C9 0.0(8) . . . . ? N1 C9 N2 C11 -0.1(7) . . . . ? N1 C9 N2 C8 -176.8(6) . . . . ? C10 C11 N2 C9 0.1(8) . . . . ? C10 C11 N2 C8 176.8(6) . . . . ? C7 C8 N2 C9 106.7(7) . . . . ? C7 C8 N2 C11 -69.4(8) . . . . ? N4 C25 N3 C26 0.5(8) . . . . ? C27 C26 N3 C25 0.3(8) . . . . ? N3 C25 N4 C27 -1.0(7) . . . . ? N3 C25 N4 C24 -176.5(6) . . . . ? C26 C27 N4 C25 1.2(8) . . . . ? C26 C27 N4 C24 176.6(6) . . . . ? C23 C24 N4 C25 104.6(7) . . . . ? C23 C24 N4 C27 -70.1(8) . . . . ? N6 C41 N5 C43 0.0(8) . . . . ? N6 C41 N5 C40 178.6(6) . . . . ? C42 C43 N5 C41 -0.2(8) . . . . ? C42 C43 N5 C40 -178.8(6) . . . . ? C39 C40 N5 C41 -104.1(8) . . . . ? C39 C40 N5 C43 74.2(8) . . . . ? N5 C41 N6 C42 0.2(8) . . . . ? C43 C42 N6 C41 -0.4(8) . . . . ? N8 C57 N7 C59 0.4(8) . . . . ? N8 C57 N7 C56 178.2(6) . . . . ? C58 C59 N7 C57 0.4(8) . . . . ? C58 C59 N7 C56 -177.5(6) . . . . ? C55 C56 N7 C57 -102.9(8) . . . . ? C55 C56 N7 C59 74.6(8) . . . . ? N7 C57 N8 C58 -1.0(8) . . . . ? C59 C58 N8 C57 1.3(8) . . . . ? C14 C12 O1 C7 -79.6(7) . . . . ? C1 C7 O1 C12 -93.3(7) . . . . ? C8 C7 O1 C12 146.7(6) . . . . ? C17 C23 O2 C28 -95.0(6) . . . . ? C24 C23 O2 C28 144.8(6) . . . . ? C30 C28 O2 C23 -79.6(7) . . . . ? C33 C39 O3 C44 91.6(6) . . . . ? C40 C39 O3 C44 -147.9(6) . . . . ? C46 C44 O3 C39 79.4(7) . . . . ? C56 C55 O4 C60 -145.3(6) . . . . ? C49 C55 O4 C60 95.1(7) . . . . ? C62 C60 O4 C55 78.3(7) . . . . ? S6 O10A O10B O11A -8.7(11) . . . . ? O10A O10B O11A O11B -7(3) . . . . ? S6 O10B O11A O11B -18(2) . . . . ? O10A O10B O11A S6 10.9(14) . . . . ? O10B O11A O11B S6 13.6(16) . . . . ? C15 C16 S1 C13 0.1(6) . . . . ? C14 C13 S1 C16 -0.3(6) . . . . ? Cl3 C13 S1 C16 178.0(5) . . . . ? C31 C32 S2 C29 0.3(6) . . . . ? C30 C29 S2 C32 -0.8(6) . . . . ? Cl6 C29 S2 C32 178.7(5) . . . . ? C46 C45 S3 C48 0.8(6) . . . . ? Cl9 C45 S3 C48 -179.4(5) . . . . ? C47 C48 S3 C45 0.2(7) . . . . ? C62 C61 S4 C64 0.0(6) . . . . ? Cl12 C61 S4 C64 -179.9(5) . . . . ? C63 C64 S4 C61 0.8(7) . . . . ? O11B O11A S6 O10B 167.8(15) . . . . ? O11B O11A S6 O12B 60.4(17) . . . . ? O10B O11A S6 O12B -107.5(9) . . . . ? O11B O11A S6 O10A 162.5(13) . . . . ? O10B O11A S6 O10A -5.3(7) . . . . ? O11B O11A S6 O12A 42.6(15) . . . . ? O10B O11A S6 O12A -125.2(6) . . . . ? O11B O11A S6 O9 -80.5(14) . . . . ? O10B O11A S6 O9 111.6(4) . . . . ? O10B O11A S6 O11B -167.8(15) . . . . ? O10A O10B S6 O11A -171.0(12) . . . . ? O10A O10B S6 O12B -46.7(12) . . . . ? O11A O10B S6 O12B 124.3(8) . . . . ? O11A O10B S6 O10A 171.0(12) . . . . ? O10A O10B S6 O12A -60.2(12) . . . . ? O11A O10B S6 O12A 110.8(7) . . . . ? O10A O10B S6 O9 79.2(10) . . . . ? O11A O10B S6 O9 -109.8(6) . . . . ? O10A O10B S6 O11B -165.3(10) . . . . ? O11A O10B S6 O11B 5.7(7) . . . . ? O12A O12B S6 O11A -55(2) . . . . ? O12A O12B S6 O10B -146.4(18) . . . . ? O12A O12B S6 O10A -170(2) . . . . ? O12A O12B S6 O9 86.0(19) . . . . ? O12A O12B S6 O11B -31(2) . . . . ? O10B O10A S6 O11A 9.5(12) . . . . ? O10B O10A S6 O12B 137.0(11) . . . . ? O10B O10A S6 O12A 133.5(9) . . . . ? O10B O10A S6 O9 -112.3(9) . . . . ? O10B O10A S6 O11B 21.0(15) . . . . ? O12B O12A S6 O11A 133.4(19) . . . . ? O12B O12A S6 O10B 40(2) . . . . ? O12B O12A S6 O10A 10(2) . . . . ? O12B O12A S6 O9 -101.1(19) . . . . ? O12B O12A S6 O11B 151(2) . . . . ? O11A O11B S6 O10B -12.4(15) . . . . ? O11A O11B S6 O12B -131.5(14) . . . . ? O11A O11B S6 O10A -24.1(18) . . . . ? O11A O11B S6 O12A -141.5(14) . . . . ? O11A O11B S6 O9 108.7(14) . . . . ? C1 C2 Cl1A Cl1B 88.5(17) . . . . ? C3 C2 Cl1A Cl1B -95.0(17) . . . . ? C1 C2 Cl1B Cl1A -103.0(16) . . . . ? C3 C2 Cl1B Cl1A 95.5(16) . . . . ? C19 C20 Cl5A Cl5B 37(2) . . . . ? C21 C20 Cl5A Cl5B -143(2) . . . . ? C19 C20 Cl5B Cl5A -148(2) . . . . ? C21 C20 Cl5B Cl5A 47(3) . . . . ? C49 C50 Cl1C Cl1D 91.1(18) . . . . ? C51 C50 Cl1C Cl1D -91.4(18) . . . . ? C49 C50 Cl1D Cl1C -100.8(19) . . . . ? C51 C50 Cl1D Cl1C 98.4(17) . . . . ?