#------------------------------------------------------------------------------ #$Date: 2024-01-06 10:01:35 +0200 (Sat, 06 Jan 2024) $ #$Revision: 288801 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247718.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_7247718 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 multicomponent crystals of the antifungal drug tioconazole and the assessment of their biopharmaceutical attributes ; _journal_issue 48 _journal_name_full CrystEngComm _journal_page_first 6758 _journal_page_last 6776 _journal_paper_doi 10.1039/D3CE00948C _journal_volume 25 _journal_year 2023 _chemical_formula_moiety 'C16 H12 Cl3 N2 O S, C16 H14 Cl3 N2 O S, O4 S, 3(H2 O), 2(O)' _chemical_formula_sum 'C32 H32 Cl6 N4 O11 S3' _chemical_formula_weight 957.49 _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 mixed _audit_creation_method SHELXL-2019/2 _audit_update_record ; 2023-09-21 deposited with the CCDC. 2023-11-14 downloaded from the CCDC. ; _cell_angle_alpha 82.360(9) _cell_angle_beta 88.440(6) _cell_angle_gamma 88.592(3) _cell_formula_units_Z 2 _cell_length_a 8.4631(3) _cell_length_b 12.0147(6) _cell_length_c 21.5955(18) _cell_measurement_reflns_used 15978 _cell_measurement_temperature 297(2) _cell_measurement_theta_max 78.8530 _cell_measurement_theta_min 2.0630 _cell_volume 2175.1(2) _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 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_environment air _diffrn_ambient_temperature 297(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 0.965 _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 39.00 94.00 0.50 0.13 -- 47.33-128.00 -15.00 110 2 \w 54.00 79.00 0.50 0.53 -- 113.25-128.00 -15.00 50 3 \w 47.00 79.00 0.50 0.53 -- 113.25-125.00 120.00 64 4 \w 84.00 109.00 0.50 0.53 -- 113.25-125.00 120.00 50 5 \w 90.00 125.00 0.50 0.53 -- 113.25-144.00 174.00 70 6 \w 50.00 103.00 0.50 0.13 -- 47.33-144.00 174.00 106 7 \w 83.00 109.00 0.50 0.53 -- 113.25-125.00 90.00 52 8 \w 45.00 81.00 0.50 0.53 -- 113.25-125.00 90.00 72 9 \w 59.00 107.00 0.50 0.53 -- 113.25-103.00 -21.12 96 10 \w 81.00 106.00 0.50 0.53 -- 113.25 -95.00 -30.00 50 11 \w 44.00 106.00 0.50 0.53 -- 113.25 -95.00 0.00 124 12 \w 52.00 86.00 0.50 0.53 -- 113.25 -95.00 120.00 68 13 \w 57.00 106.00 0.50 0.53 -- 113.25 -95.00-120.00 98 14 \w 80.00 106.00 0.50 0.53 -- 113.25 -95.00-150.00 52 15 \w 43.00 69.00 0.50 0.53 -- 113.25 -95.00-150.00 52 16 \w 44.00 108.00 0.50 0.53 -- 113.25-108.00-177.64 128 17 \w 75.00 106.00 0.50 0.53 -- 113.25 -95.00-180.00 62 18 \w 46.00 106.00 0.50 0.53 -- 113.25 -95.00 -90.00 120 19 \w 46.00 92.00 0.50 0.53 -- 113.25 -95.00 -60.00 92 20 \w 45.00 73.00 0.50 0.53 -- 113.25 -95.00 30.00 56 21 \w 77.00 106.00 0.50 0.53 -- 113.25 -95.00 60.00 58 22 \w 53.00 98.00 0.50 0.53 -- 113.25 -95.00 150.00 90 23 \w 43.00 69.00 0.50 0.53 -- 113.25 -61.00 150.00 52 24 \w 44.00 72.00 0.50 0.53 -- 113.25 -61.00 90.00 56 25 \w 42.00 68.00 0.50 0.53 -- 113.25 -61.00 30.00 52 26 \w 43.00 71.00 0.50 0.53 -- 113.25 -61.00 -60.00 56 27 \w 44.00 73.00 0.50 0.53 -- 113.25 -61.00-150.00 58 28 \w 46.00 71.00 0.50 0.53 -- 113.25 -61.00-180.00 50 29 \w 100.00 173.00 0.50 0.53 -- 113.25 15.00 -60.00 146 30 \w 110.00 178.00 0.50 0.53 -- 113.25 30.00-120.00 136 31 \w 102.00 157.00 0.50 0.53 -- 113.25 30.00 30.00 110 32 \w 124.00 150.00 0.50 0.53 -- 113.25 45.00 60.00 52 33 \w 104.00 139.00 0.50 0.53 -- 113.25 30.00 120.00 70 34 \w 102.00 170.00 0.50 0.53 -- 113.25 45.00 150.00 136 35 \w 101.00 144.00 0.50 0.53 -- 113.25 15.00 0.00 86 36 \w 100.00 158.00 0.50 0.53 -- 113.25 15.00 -30.00 116 37 \w 106.00 178.00 0.50 0.53 -- 113.25 15.00-150.00 144 38 \w 102.00 127.00 0.50 0.53 -- 113.25 144.00-131.00 50 39 \w 119.00 159.00 0.50 0.53 -- 113.25 128.00 59.00 80 40 \w -26.00 9.00 0.50 0.13 -- 47.33 -19.00 0.00 70 41 \w -118.00 -30.00 0.50 0.13 -- -47.33 -77.00-120.00 176 42 \w -141.00-116.00 0.50 0.53 -- -91.75-128.00 -15.00 50 43 \w -99.00 -73.00 0.50 0.13 -- -47.33-128.00 -15.00 52 44 \w -116.00 -67.00 0.50 0.13 -- -47.33-144.00 174.00 98 45 \w -131.00-106.00 0.50 0.53 -- -91.75-144.00 174.00 50 46 \w -164.00-138.00 0.50 0.53 -- -91.75 -30.00 30.00 52 47 \w -49.00 -21.00 0.50 0.53 -- -91.75 45.00-180.00 56 48 \w -22.00 28.00 0.50 0.13 -- -47.33 19.00-180.00 100 49 \w -8.00 25.00 0.50 0.13 -- -47.33 19.00-150.00 66 50 \w -24.00 14.00 0.50 0.13 -- -47.33 19.00 0.00 76 51 \w -41.00 23.00 0.50 0.13 -- -47.33 38.00 90.00 128 52 \w -74.00 -49.00 0.50 0.53 -- -91.75 128.00 59.00 50 53 \w -47.00 -22.00 0.50 0.13 -- -47.33 128.00 59.00 50 54 \w -86.00 -61.00 0.50 0.13 -- -47.33 144.00-131.00 50 55 \w -86.00 -61.00 0.50 0.53 -- -91.75 144.00-131.00 50 ; _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 -0.0706956000 _diffrn_orient_matrix_UB_12 -0.0201951000 _diffrn_orient_matrix_UB_13 0.0669392000 _diffrn_orient_matrix_UB_21 0.1619271000 _diffrn_orient_matrix_UB_22 0.0224801000 _diffrn_orient_matrix_UB_23 0.0262431000 _diffrn_orient_matrix_UB_31 -0.0442397000 _diffrn_orient_matrix_UB_32 0.1258222000 _diffrn_orient_matrix_UB_33 -0.0037462000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_unetI/netI 0.0789 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 29542 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 79.883 _diffrn_reflns_theta_min 2.065 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.451 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.36691 _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 1.462 _exptl_crystal_description plate _exptl_crystal_F_000 980 _exptl_crystal_size_max 0.270 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.435 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.093 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 600 _refine_ls_number_reflns 9156 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0860 _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^)+(0.1756P)^2^+0.2368P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2464 _refine_ls_wR_factor_ref 0.2716 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6864 _reflns_number_total 9156 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce00948c2.cif _cod_data_source_block TCZ-SULH _cod_depositor_comments 'Adding full bibliography for 7247709--7247724.cif.' _cod_database_code 7247718 _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 0.321 _shelx_estimated_absorpt_t_max 0.899 _oxdiff_exptl_absorpt_empirical_full_min 0.344 _oxdiff_exptl_absorpt_empirical_full_max 4.021 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL shelxt_a.res in P-1 shelx.res created by SHELXL-2019/2 at 14:49:36 on 21-Sep-2023 CELL 1.54184 8.4631 12.0147 21.5955 82.360 88.440 88.592 ZERR 2.00 0.0003 0.0006 0.0018 0.009 0.006 0.003 LATT 1 SFAC C H N O S CL UNIT 64 64 8 22 6 12 MERG 2 OMIT 4 8 0 DFIX 0.900 0.020 O11 H11A DFIX 0.900 0.020 O11 H11B DANG 1.200 0.040 H11B O11 H11B H11A DFIX 0.900 0.020 O10 H10A DFIX 0.900 0.020 O10 H10B DANG 1.200 0.040 H10A O10 H10A H10B FMAP 2 PLAN 5 SIZE 0.020 0.100 0.270 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP 24.00 WGHT 0.175600 0.236800 FVAR 3.39732 0.50231 0.36172 C1 1 0.296845 0.984058 0.786195 11.00000 0.05652 0.03069 = 0.07383 -0.01437 0.00856 0.00465 C2 1 0.212005 1.082136 0.793206 11.00000 0.05862 0.03140 = 0.09066 -0.01437 0.01265 0.00647 C3 1 0.220312 1.133282 0.846971 11.00000 0.07948 0.04304 = 0.09851 -0.02694 0.02652 -0.00031 AFIX 43 H3 2 0.161914 1.198439 0.851440 11.00000 -1.20000 AFIX 0 C4 1 0.317266 1.084766 0.893268 11.00000 0.09151 0.06264 = 0.07866 -0.03053 0.02133 -0.00692 C5 1 0.403315 0.986710 0.888625 11.00000 0.08829 0.06630 = 0.06974 -0.01284 0.01131 0.00205 AFIX 43 H5 2 0.466772 0.954456 0.920976 11.00000 -1.20000 AFIX 0 C6 1 0.392032 0.938063 0.834301 11.00000 0.06382 0.04491 = 0.07881 -0.01602 0.00881 0.00831 AFIX 43 H6 2 0.450147 0.872661 0.830130 11.00000 -1.20000 AFIX 0 C7 1 0.288475 0.929588 0.726621 11.00000 0.05162 0.03262 = 0.08271 -0.01583 -0.00143 0.01108 AFIX 13 H7 2 0.181401 0.939035 0.710272 11.00000 -1.20000 AFIX 0 C8 1 0.405676 0.985583 0.678658 11.00000 0.05857 0.04053 = 0.07127 -0.01801 -0.00446 0.00323 AFIX 23 H8A 2 0.379755 1.065147 0.670150 11.00000 -1.20000 H8B 2 0.511145 0.977587 0.695407 11.00000 -1.20000 AFIX 0 C9 1 0.527760 0.904908 0.588447 11.00000 0.07306 0.06264 = 0.07364 -0.01915 -0.00612 0.01122 AFIX 43 H9 2 0.632220 0.910435 0.599784 11.00000 -1.20000 AFIX 0 C10 1 0.321614 0.869758 0.538279 11.00000 0.10282 0.08873 = 0.08720 -0.03784 -0.02504 -0.00249 AFIX 43 H10 2 0.257578 0.845967 0.508485 11.00000 -1.20000 AFIX 0 C11 1 0.272539 0.914270 0.588545 11.00000 0.06978 0.10687 = 0.11079 -0.05362 -0.01989 0.00798 AFIX 43 H11 2 0.168124 0.928440 0.600181 11.00000 -1.20000 AFIX 0 C12 1 0.201775 0.746870 0.763088 11.00000 0.05023 0.03702 = 0.15810 -0.02071 0.01421 0.00579 AFIX 23 H12A 2 0.111953 0.759561 0.735890 11.00000 -1.20000 H12B 2 0.170365 0.767305 0.803685 11.00000 -1.20000 AFIX 0 C13 1 0.273023 0.558968 0.824338 11.00000 0.06513 0.04804 = 0.10555 -0.02323 0.01551 -0.00306 C14 1 0.252918 0.626041 0.769399 11.00000 0.04617 0.03873 = 0.10991 -0.02515 0.00579 0.00235 C15 1 0.286029 0.564593 0.718377 11.00000 0.05031 0.06366 = 0.10147 -0.02659 -0.00755 0.00233 AFIX 43 H15 2 0.280530 0.595658 0.676666 11.00000 -1.20000 AFIX 0 C16 1 0.326767 0.454946 0.737496 11.00000 0.05410 0.05431 = 0.13971 -0.05400 0.00163 0.00504 AFIX 43 H16 2 0.350877 0.402894 0.710218 11.00000 -1.20000 AFIX 0 C17 1 0.805926 0.364891 0.823480 11.00000 0.05357 0.03675 = 0.05963 -0.01137 -0.00260 0.00731 C18 1 0.738014 0.260235 0.834693 11.00000 0.05719 0.03861 = 0.07203 -0.01762 0.00082 0.00519 C19 1 0.759865 0.189574 0.889935 11.00000 0.07398 0.04276 = 0.08492 -0.00299 0.00820 0.00427 AFIX 43 H19 2 0.713041 0.119649 0.896818 11.00000 -1.20000 AFIX 0 C20 1 0.852477 0.225314 0.934363 11.00000 0.08345 0.06340 = 0.07021 0.00469 0.00212 0.01404 C21 1 0.924326 0.326912 0.925358 11.00000 0.08017 0.06721 = 0.06874 -0.01031 -0.01059 0.00263 AFIX 43 H21 2 0.988493 0.348646 0.955720 11.00000 -1.20000 AFIX 0 C22 1 0.899496 0.396831 0.870013 11.00000 0.06598 0.04584 = 0.07046 -0.01190 -0.01094 0.00044 AFIX 43 H22 2 0.946334 0.466776 0.863711 11.00000 -1.20000 AFIX 0 C23 1 0.776188 0.445687 0.764092 11.00000 0.04921 0.03000 = 0.06429 -0.01352 -0.00793 0.00426 AFIX 13 H23 2 0.664105 0.444109 0.754046 11.00000 -1.20000 AFIX 0 C24 1 0.876459 0.415013 0.708337 11.00000 0.05569 0.04363 = 0.06045 -0.01270 -0.00724 0.01319 AFIX 23 H24A 2 0.987782 0.422639 0.716084 11.00000 -1.20000 H24B 2 0.858705 0.337719 0.702408 11.00000 -1.20000 AFIX 0 C25 1 0.711480 0.476644 0.616205 11.00000 0.05889 0.05085 = 0.06280 -0.01585 -0.00933 -0.00053 AFIX 43 H25 2 0.645788 0.415022 0.620622 11.00000 -1.20000 AFIX 0 C26 1 0.817283 0.636905 0.580761 11.00000 0.08422 0.06505 = 0.07414 0.00992 -0.01054 -0.01741 AFIX 43 H26 2 0.836488 0.704971 0.556097 11.00000 -1.20000 AFIX 0 C27 1 0.898384 0.591886 0.630245 11.00000 0.07277 0.07093 = 0.07925 0.00282 -0.01471 -0.02389 AFIX 43 H27 2 0.984511 0.623310 0.646781 11.00000 -1.20000 AFIX 0 C28 1 0.687771 0.617530 0.796677 11.00000 0.05606 0.04340 = 0.09855 -0.02989 0.00088 0.00714 C29A 1 0.790614 0.753266 0.871431 21.00000 0.08115 0.05824 = 0.06626 -0.03988 -0.03112 0.02594 C29B 1 0.778492 0.765775 0.849925 -21.00000 0.07441 0.08246 = 0.07615 -0.03459 -0.02792 0.02773 C30A 1 0.750382 0.739271 0.793049 21.00000 0.05460 C30B 1 0.744790 0.724380 0.814080 -21.00000 0.03954 C31A 1 0.766017 0.813805 0.765156 21.00000 0.06121 0.02963 = 0.06610 0.00905 0.00810 0.01160 C31B 1 0.770085 0.828517 0.741515 -21.00000 0.07121 0.04571 = 0.12968 0.03300 0.00746 0.00511 C32A 1 0.828683 0.912841 0.787431 21.00000 0.06850 0.04183 = 0.10545 -0.02591 0.00009 0.00854 C32B 1 0.815468 0.913832 0.759796 -21.00000 0.06691 0.05275 = 0.18493 -0.01103 -0.01187 0.00476 N1 3 0.403335 0.935377 0.619956 11.00000 0.06173 0.04489 = 0.07145 -0.02128 -0.00959 0.01112 N2 3 0.481178 0.865112 0.538040 11.00000 0.09952 0.06041 = 0.07095 -0.02463 -0.00685 0.01367 N3 3 0.831672 0.490175 0.652607 11.00000 0.05076 0.04415 = 0.05926 -0.01249 -0.00691 0.00205 N4 3 0.700277 0.563666 0.573229 11.00000 0.06464 0.06246 = 0.05843 -0.01186 -0.01141 0.00548 O1 4 0.330140 0.813269 0.737539 11.00000 0.05009 0.02781 = 0.09562 -0.01928 0.00280 0.00818 O2 4 0.816168 0.557663 0.770491 11.00000 0.05215 0.03191 = 0.07092 -0.01378 -0.00233 0.00421 O3 4 0.663647 0.803409 0.445917 11.00000 0.07160 0.05874 = 0.08050 -0.02815 -0.00512 -0.01241 O4 4 0.525976 0.629444 0.469849 11.00000 0.05804 0.06838 = 0.06445 0.00709 -0.00834 -0.01013 O5 4 0.770149 0.636798 0.409791 11.00000 0.05830 0.05455 = 0.09204 -0.01119 -0.00456 0.00439 O6 4 0.534107 0.724944 0.364411 11.00000 0.06596 0.05750 = 0.05919 -0.00428 -0.01158 -0.00107 O7 4 0.745682 0.141042 0.628012 11.00000 0.09412 0.09259 = 0.12766 -0.00048 0.01346 0.02121 O8 4 0.886625 0.935018 0.616499 11.00000 0.11457 0.14272 = 0.24993 -0.00604 0.02019 0.00347 O9A 4 0.902123 0.896685 0.535331 31.00000 0.12196 0.07073 = 0.16898 -0.02102 0.00216 -0.01081 O9B 4 0.933842 0.890606 0.490477 -31.00000 0.08264 0.06486 = 0.16026 -0.01913 -0.01130 -0.00205 O10 4 0.059892 0.705866 0.445761 11.00000 0.06470 0.09896 = 0.14462 -0.00734 -0.01185 -0.01317 O11 4 0.236778 0.595520 0.542334 11.00000 0.07366 0.06387 = 0.11961 -0.01723 0.00795 0.00846 S1 5 0.328558 0.424301 0.815967 11.00000 0.08013 0.03741 = 0.13262 -0.00976 0.01724 0.00376 S2A 5 0.847708 0.887065 0.866477 21.00000 0.10579 0.05536 = 0.12214 -0.04981 -0.01504 0.00619 S2B 5 0.846916 0.906388 0.839044 -21.00000 0.07825 0.07316 = 0.25893 -0.09469 -0.00115 0.00213 S3 5 0.624234 0.698759 0.421721 11.00000 0.05088 0.04209 = 0.05438 -0.00745 -0.00667 -0.00159 CL1 6 0.093651 1.147074 0.733635 11.00000 0.08295 0.04288 = 0.12843 -0.01506 -0.00986 0.02564 CL2 6 0.333415 1.150956 0.959491 11.00000 0.15417 0.11118 = 0.09802 -0.06050 0.02306 -0.01075 CL3 6 0.248489 0.596594 0.898203 11.00000 0.16010 0.12482 = 0.11656 -0.05135 0.03956 -0.00926 CL4 6 0.621042 0.214914 0.778566 11.00000 0.08043 0.04503 = 0.09470 -0.02461 -0.00867 -0.00661 CL5 6 0.878620 0.137849 1.005234 11.00000 0.14464 0.10996 = 0.09032 0.03714 -0.00982 0.00045 CL6A 6 0.779066 0.667027 0.938244 21.00000 0.16757 0.07758 = 0.07250 -0.02839 -0.01876 0.01672 CL6B 6 0.772073 0.693796 0.922887 -21.00000 0.23255 0.21219 = 0.10010 -0.07182 -0.03081 0.04663 H2N 2 0.559304 0.835172 0.513714 11.00000 0.09418 H4N 2 0.624483 0.580719 0.546872 11.00000 0.10940 H7A 2 0.647681 0.173740 0.630859 11.00000 0.08403 H7B 2 0.809995 0.193320 0.613230 11.00000 0.11471 H10A 2 -0.033684 0.674998 0.432065 11.00000 0.09526 H10B 2 -0.006905 0.764446 0.449417 11.00000 0.29033 H11A 2 0.305719 0.623346 0.512303 11.00000 0.21632 H11B 2 0.173776 0.584563 0.507632 11.00000 0.27182 H28A 2 0.583776 0.614503 0.770928 11.00000 0.07131 H28B 2 0.653360 0.580348 0.841795 11.00000 0.07302 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.2716, GooF = S = 1.095, Restrained GooF = 1.100 for all data REM R1 = 0.0860 for 6864 Fo > 4sig(Fo) and 0.1016 for all 9156 data REM 600 parameters refined using 8 restraints END WGHT 0.1756 0.2368 REM Highest difference peak 0.435, deepest hole -0.673, 1-sigma level 0.093 Q1 1 0.0842 1.1277 0.7721 11.00000 0.05 0.43 Q2 1 0.6292 0.2034 0.8190 11.00000 0.05 0.41 Q3 1 0.3367 0.4224 0.8653 11.00000 0.05 0.39 Q4 1 0.7207 0.7750 0.4212 11.00000 0.05 0.38 Q5 1 0.3514 0.6177 0.9078 11.00000 0.05 0.37 ; _shelx_res_checksum 89338 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 C1 C 0.2968(4) 0.9841(3) 0.78619(18) 0.0533(7) Uani 1 1 d . . . . . C2 C 0.2120(5) 1.0821(3) 0.7932(2) 0.0600(9) Uani 1 1 d . . . . . C3 C 0.2203(6) 1.1333(3) 0.8470(2) 0.0726(12) Uani 1 1 d . . . . . H3 H 0.161914 1.198439 0.851440 0.087 Uiso 1 1 calc R U . . . C4 C 0.3173(6) 1.0848(4) 0.8933(2) 0.0760(12) Uani 1 1 d . . . . . C5 C 0.4033(6) 0.9867(4) 0.8886(2) 0.0747(11) Uani 1 1 d . . . . . H5 H 0.466772 0.954456 0.920976 0.090 Uiso 1 1 calc R U . . . C6 C 0.3920(5) 0.9381(3) 0.8343(2) 0.0622(9) Uani 1 1 d . . . . . H6 H 0.450147 0.872661 0.830130 0.075 Uiso 1 1 calc R U . . . C7 C 0.2885(4) 0.9296(3) 0.72662(19) 0.0551(8) Uani 1 1 d . . . . . H7 H 0.181401 0.939035 0.710272 0.066 Uiso 1 1 calc R U . . . C8 C 0.4057(4) 0.9856(3) 0.67866(18) 0.0558(8) Uani 1 1 d . . . . . H8A H 0.379755 1.065147 0.670150 0.067 Uiso 1 1 calc R U . . . H8B H 0.511145 0.977587 0.695407 0.067 Uiso 1 1 calc R U . . . C9 C 0.5278(6) 0.9049(4) 0.5884(2) 0.0690(10) Uani 1 1 d . . . . . H9 H 0.632220 0.910435 0.599784 0.083 Uiso 1 1 calc R U . . . C10 C 0.3216(7) 0.8698(5) 0.5383(3) 0.0901(15) Uani 1 1 d . . . . . H10 H 0.257578 0.845967 0.508485 0.108 Uiso 1 1 calc R U . . . C11 C 0.2725(6) 0.9143(5) 0.5885(3) 0.0921(16) Uani 1 1 d . . . . . H11 H 0.168124 0.928440 0.600181 0.111 Uiso 1 1 calc R U . . . C12 C 0.2018(5) 0.7469(3) 0.7631(3) 0.0815(15) Uani 1 1 d . . . . . H12A H 0.111953 0.759561 0.735890 0.098 Uiso 1 1 calc R U . . . H12B H 0.170365 0.767305 0.803685 0.098 Uiso 1 1 calc R U . . . C13 C 0.2730(5) 0.5590(3) 0.8243(3) 0.0720(11) Uani 1 1 d . . . . . C14 C 0.2529(4) 0.6260(3) 0.7694(2) 0.0638(10) Uani 1 1 d . . . . . C15 C 0.2860(5) 0.5646(4) 0.7184(3) 0.0704(10) Uani 1 1 d . . . . . H15 H 0.280530 0.595658 0.676666 0.084 Uiso 1 1 calc R U . . . C16 C 0.3268(5) 0.4549(4) 0.7375(3) 0.0792(14) Uani 1 1 d . . . . . H16 H 0.350877 0.402894 0.710218 0.095 Uiso 1 1 calc R U . . . C17 C 0.8059(4) 0.3649(3) 0.82348(16) 0.0496(7) Uani 1 1 d . . . . . C18 C 0.7380(4) 0.2602(3) 0.83469(18) 0.0552(8) Uani 1 1 d . . . . . C19 C 0.7599(5) 0.1896(3) 0.8899(2) 0.0680(10) Uani 1 1 d . . . . . H19 H 0.713041 0.119649 0.896818 0.082 Uiso 1 1 calc R U . . . C20 C 0.8525(6) 0.2253(4) 0.9344(2) 0.0739(11) Uani 1 1 d . . . . . C21 C 0.9243(6) 0.3269(4) 0.9254(2) 0.0718(10) Uani 1 1 d . . . . . H21 H 0.988493 0.348646 0.955720 0.086 Uiso 1 1 calc R U . . . C22 C 0.8995(5) 0.3968(3) 0.87001(19) 0.0602(8) Uani 1 1 d . . . . . H22 H 0.946334 0.466776 0.863711 0.072 Uiso 1 1 calc R U . . . C23 C 0.7762(4) 0.4457(2) 0.76409(16) 0.0471(7) Uani 1 1 d . . . . . H23 H 0.664105 0.444109 0.754046 0.057 Uiso 1 1 calc R U . . . C24 C 0.8765(4) 0.4150(3) 0.70834(16) 0.0529(7) Uani 1 1 d . . . . . H24A H 0.987782 0.422639 0.716084 0.063 Uiso 1 1 calc R U . . . H24B H 0.858705 0.337719 0.702408 0.063 Uiso 1 1 calc R U . . . C25 C 0.7115(4) 0.4766(3) 0.61620(17) 0.0566(8) Uani 1 1 d . . . . . H25 H 0.645788 0.415022 0.620622 0.068 Uiso 1 1 calc R U . . . C26 C 0.8173(6) 0.6369(4) 0.5808(2) 0.0758(11) Uani 1 1 d . . . . . H26 H 0.836488 0.704971 0.556097 0.091 Uiso 1 1 calc R U . . . C27 C 0.8984(6) 0.5919(4) 0.6302(2) 0.0749(11) Uani 1 1 d . . . . . H27 H 0.984511 0.623310 0.646781 0.090 Uiso 1 1 calc R U . . . C28 C 0.6878(5) 0.6175(3) 0.7967(2) 0.0643(10) Uani 1 1 d . . . . . C29A C 0.791(3) 0.7533(16) 0.8714(9) 0.066(4) Uani 0.50(3) 1 d . . P . . C29B C 0.778(3) 0.766(2) 0.8499(11) 0.076(4) Uani 0.50(3) 1 d . . P . . C30A C 0.7504(9) 0.7393(9) 0.7930(7) 0.055(3) Uiso 0.50(3) 1 d . . P . . C30B C 0.7448(7) 0.7244(6) 0.8141(5) 0.040(2) Uiso 0.50(3) 1 d . . P . . C31A C 0.7660(19) 0.8138(13) 0.7652(6) 0.054(3) Uani 0.50(3) 1 d . . P . . C31B C 0.770(2) 0.8285(18) 0.7415(14) 0.087(6) Uani 0.50(3) 1 d . . P . . C32A C 0.829(3) 0.9128(18) 0.7874(10) 0.071(4) Uani 0.50(3) 1 d . . P . . C32B C 0.815(3) 0.914(2) 0.7598(18) 0.102(8) Uani 0.50(3) 1 d . . P . . N1 N 0.4033(4) 0.9354(2) 0.61996(16) 0.0582(7) Uani 1 1 d . . . . . N2 N 0.4812(6) 0.8651(3) 0.53804(19) 0.0757(10) Uani 1 1 d . . . . . N3 N 0.8317(3) 0.4902(2) 0.65261(14) 0.0508(6) Uani 1 1 d . . . . . N4 N 0.7003(4) 0.5637(3) 0.57323(15) 0.0614(7) Uani 1 1 d . . . . . O1 O 0.3301(3) 0.81327(17) 0.73754(14) 0.0571(6) Uani 1 1 d . . . . . O2 O 0.8162(3) 0.55766(17) 0.77049(12) 0.0511(5) Uani 1 1 d . . . . . O3 O 0.6636(4) 0.8034(2) 0.44592(15) 0.0683(7) Uani 1 1 d . . . . . O4 O 0.5260(3) 0.6294(2) 0.46985(13) 0.0648(7) Uani 1 1 d . . . . . O5 O 0.7701(3) 0.6368(2) 0.40979(15) 0.0682(7) Uani 1 1 d . . . . . O6 O 0.5341(3) 0.7249(2) 0.36441(12) 0.0610(6) Uani 1 1 d . . . . . O7 O 0.7457(7) 0.1410(4) 0.6280(3) 0.1067(14) Uani 1 1 d . . . . . O8 O 0.8866(8) 0.9350(6) 0.6165(5) 0.171(3) Uani 1 1 d . . . . . O9A O 0.902(3) 0.8967(12) 0.535(2) 0.120(10) Uani 0.36(4) 1 d . . P . . O9B O 0.9338(11) 0.8906(6) 0.4905(11) 0.102(5) Uani 0.64(4) 1 d . . P . . O10 O 0.0599(5) 0.7059(4) 0.4458(3) 0.1032(13) Uani 1 1 d D . . . . O11 O 0.2368(4) 0.5955(3) 0.5423(2) 0.0856(10) Uani 1 1 d D . . . . S1 S 0.32856(15) 0.42430(8) 0.81597(8) 0.0840(4) Uani 1 1 d . . . . . S2A S 0.8477(13) 0.8871(7) 0.8665(4) 0.0909(16) Uani 0.50(3) 1 d . . P . . S2B S 0.8469(9) 0.9064(11) 0.8390(14) 0.130(6) Uani 0.50(3) 1 d . . P . . S3 S 0.62423(9) 0.69876(6) 0.42172(4) 0.0489(2) Uani 1 1 d . . . . . Cl1 Cl 0.09365(14) 1.14707(8) 0.73364(7) 0.0847(4) Uani 1 1 d . . . . . Cl2 Cl 0.3334(3) 1.15096(16) 0.95949(8) 0.1173(6) Uani 1 1 d . . . . . Cl3 Cl 0.2485(3) 0.59659(19) 0.89820(10) 0.1313(7) Uani 1 1 d . . . . . Cl4 Cl 0.62104(13) 0.21491(8) 0.77857(6) 0.0718(3) Uani 1 1 d . . . . . Cl5 Cl 0.8786(3) 0.13785(16) 1.00523(8) 0.1194(6) Uani 1 1 d . . . . . Cl6A Cl 0.7791(13) 0.6670(5) 0.9382(4) 0.104(2) Uani 0.50(3) 1 d . . P . . Cl6B Cl 0.772(2) 0.6938(18) 0.9229(8) 0.177(5) Uani 0.50(3) 1 d . . P . . H2N H 0.559(8) 0.835(5) 0.514(3) 0.094(18) Uiso 1 1 d . . . . . H4N H 0.624(9) 0.581(6) 0.547(3) 0.11(2) Uiso 1 1 d . . . . . H7A H 0.648(8) 0.174(5) 0.631(3) 0.084(16) Uiso 1 1 d . . . . . H7B H 0.810(10) 0.193(7) 0.613(4) 0.11(3) Uiso 1 1 d . . . . . H10A H -0.034(5) 0.675(5) 0.432(3) 0.095(18) Uiso 1 1 d D . . . . H10B H -0.007(9) 0.764(7) 0.449(8) 0.29(9) Uiso 1 1 d D . . . . H11A H 0.306(12) 0.623(11) 0.512(4) 0.22(6) Uiso 1 1 d D . . . . H11B H 0.174(15) 0.585(15) 0.508(4) 0.27(8) Uiso 1 1 d D . . . . H28A H 0.584(6) 0.615(4) 0.771(2) 0.071(13) Uiso 1 1 d . . . . . H28B H 0.653(6) 0.580(4) 0.842(3) 0.073(14) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0565(18) 0.0307(14) 0.074(2) -0.0144(13) 0.0086(15) 0.0047(12) C2 0.0586(19) 0.0314(15) 0.091(3) -0.0144(15) 0.0127(17) 0.0065(13) C3 0.079(3) 0.0430(19) 0.099(3) -0.0269(19) 0.027(2) -0.0003(17) C4 0.092(3) 0.063(2) 0.079(3) -0.031(2) 0.021(2) -0.007(2) C5 0.088(3) 0.066(2) 0.070(2) -0.0128(19) 0.011(2) 0.002(2) C6 0.064(2) 0.0449(18) 0.079(2) -0.0160(16) 0.0088(17) 0.0083(15) C7 0.0516(17) 0.0326(15) 0.083(2) -0.0158(14) -0.0014(15) 0.0111(12) C8 0.0586(18) 0.0405(16) 0.071(2) -0.0180(14) -0.0045(15) 0.0032(13) C9 0.073(2) 0.063(2) 0.074(2) -0.0191(18) -0.0061(18) 0.0112(18) C10 0.103(4) 0.089(3) 0.087(3) -0.038(3) -0.025(3) -0.002(3) C11 0.070(3) 0.107(4) 0.111(4) -0.054(3) -0.020(3) 0.008(3) C12 0.050(2) 0.0370(18) 0.158(5) -0.021(2) 0.014(2) 0.0058(14) C13 0.065(2) 0.0480(19) 0.106(3) -0.023(2) 0.016(2) -0.0031(16) C14 0.0462(17) 0.0387(17) 0.110(3) -0.0251(18) 0.0058(17) 0.0024(12) C15 0.0503(19) 0.064(2) 0.101(3) -0.027(2) -0.0075(18) 0.0023(16) C16 0.054(2) 0.054(2) 0.140(4) -0.054(3) 0.002(2) 0.0050(16) C17 0.0536(17) 0.0368(14) 0.0596(17) -0.0114(12) -0.0026(13) 0.0073(12) C18 0.0572(18) 0.0386(15) 0.072(2) -0.0176(14) 0.0008(15) 0.0052(13) C19 0.074(2) 0.0428(18) 0.085(3) -0.0030(17) 0.0082(19) 0.0043(16) C20 0.083(3) 0.063(2) 0.070(2) 0.0047(18) 0.002(2) 0.014(2) C21 0.080(3) 0.067(2) 0.069(2) -0.0103(18) -0.0106(19) 0.003(2) C22 0.066(2) 0.0458(17) 0.070(2) -0.0119(15) -0.0109(16) 0.0004(14) C23 0.0492(15) 0.0300(13) 0.0643(17) -0.0135(12) -0.0079(13) 0.0043(11) C24 0.0557(17) 0.0436(16) 0.0604(18) -0.0127(13) -0.0072(13) 0.0132(13) C25 0.0589(19) 0.0508(18) 0.0628(19) -0.0158(14) -0.0093(15) -0.0005(14) C26 0.084(3) 0.065(2) 0.074(2) 0.010(2) -0.011(2) -0.017(2) C27 0.073(3) 0.071(3) 0.079(3) 0.003(2) -0.015(2) -0.024(2) C28 0.0561(19) 0.0434(17) 0.099(3) -0.0299(18) 0.0009(18) 0.0071(14) C29A 0.081(7) 0.058(7) 0.066(10) -0.040(7) -0.031(7) 0.026(5) C29B 0.074(7) 0.082(8) 0.076(11) -0.035(9) -0.028(8) 0.028(5) C31A 0.061(5) 0.030(6) 0.066(6) 0.009(5) 0.008(5) 0.012(4) C31B 0.071(6) 0.046(6) 0.130(17) 0.033(10) 0.007(10) 0.005(4) C32A 0.068(9) 0.042(5) 0.105(11) -0.026(9) 0.000(9) 0.009(5) C32B 0.067(7) 0.053(7) 0.18(3) -0.011(15) -0.012(15) 0.005(5) N1 0.0617(17) 0.0449(14) 0.0714(18) -0.0213(13) -0.0096(13) 0.0111(12) N2 0.100(3) 0.060(2) 0.071(2) -0.0246(16) -0.0068(19) 0.0137(18) N3 0.0508(14) 0.0442(13) 0.0593(15) -0.0125(11) -0.0069(11) 0.0021(10) N4 0.0646(18) 0.0625(18) 0.0584(16) -0.0119(13) -0.0114(13) 0.0055(14) O1 0.0501(12) 0.0278(10) 0.0956(18) -0.0193(10) 0.0028(11) 0.0082(8) O2 0.0522(12) 0.0319(10) 0.0709(14) -0.0138(9) -0.0023(10) 0.0042(8) O3 0.0716(16) 0.0587(15) 0.0805(17) -0.0281(13) -0.0051(13) -0.0124(12) O4 0.0580(14) 0.0684(16) 0.0644(15) 0.0071(12) -0.0083(11) -0.0101(12) O5 0.0583(15) 0.0545(14) 0.092(2) -0.0112(13) -0.0046(13) 0.0044(11) O6 0.0660(15) 0.0575(14) 0.0592(13) -0.0043(11) -0.0116(11) -0.0011(11) O7 0.094(3) 0.093(3) 0.128(4) 0.000(3) 0.013(3) 0.021(2) O8 0.115(4) 0.143(5) 0.250(9) -0.006(6) 0.020(5) 0.003(4) O9A 0.122(11) 0.071(7) 0.17(3) -0.021(9) 0.002(13) -0.011(7) O9B 0.083(5) 0.065(4) 0.160(14) -0.019(4) -0.011(5) -0.002(3) O10 0.065(2) 0.099(3) 0.145(4) -0.007(3) -0.012(2) -0.0132(19) O11 0.074(2) 0.0639(18) 0.120(3) -0.0172(18) 0.0080(19) 0.0085(15) S1 0.0801(7) 0.0374(5) 0.1326(11) -0.0098(5) 0.0172(7) 0.0038(4) S2A 0.106(3) 0.055(2) 0.122(4) -0.050(2) -0.015(2) 0.0062(16) S2B 0.078(2) 0.073(5) 0.259(16) -0.095(9) -0.001(7) 0.002(2) S3 0.0509(4) 0.0421(4) 0.0544(4) -0.0075(3) -0.0067(3) -0.0016(3) Cl1 0.0829(7) 0.0429(5) 0.1284(10) -0.0151(5) -0.0099(6) 0.0256(4) Cl2 0.1542(15) 0.1112(11) 0.0980(10) -0.0605(9) 0.0231(9) -0.0107(10) Cl3 0.1601(18) 0.1248(14) 0.1166(13) -0.0513(11) 0.0396(12) -0.0093(12) Cl4 0.0804(6) 0.0450(5) 0.0947(7) -0.0246(4) -0.0087(5) -0.0066(4) Cl5 0.1446(14) 0.1100(12) 0.0903(9) 0.0371(9) -0.0098(9) 0.0004(10) Cl6A 0.168(4) 0.078(3) 0.072(3) -0.0284(18) -0.019(2) 0.017(2) Cl6B 0.233(8) 0.212(11) 0.100(7) -0.072(7) -0.031(6) 0.047(9) 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 118.2(4) . . ? C6 C1 C7 120.6(3) . . ? C2 C1 C7 121.2(3) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 Cl1 117.5(3) . . ? C1 C2 Cl1 120.8(3) . . ? C4 C3 C2 117.9(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 122.5(4) . . ? C3 C4 Cl2 118.2(3) . . ? C5 C4 Cl2 119.3(4) . . ? C4 C5 C6 117.9(5) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C1 C6 C5 121.8(3) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O1 C7 C8 107.6(3) . . ? O1 C7 C1 111.3(3) . . ? C8 C7 C1 108.9(3) . . ? O1 C7 H7 109.7 . . ? C8 C7 H7 109.7 . . ? C1 C7 H7 109.7 . . ? N1 C8 C7 111.2(3) . . ? N1 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N1 C9 N2 109.1(4) . . ? N1 C9 H9 125.5 . . ? N2 C9 H9 125.5 . . ? C11 C10 N2 107.8(4) . . ? C11 C10 H10 126.1 . . ? N2 C10 H10 126.1 . . ? C10 C11 N1 107.2(5) . . ? C10 C11 H11 126.4 . . ? N1 C11 H11 126.4 . . ? O1 C12 C14 108.6(3) . . ? O1 C12 H12A 110.0 . . ? C14 C12 H12A 110.0 . . ? O1 C12 H12B 110.0 . . ? C14 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? C14 C13 S1 113.8(3) . . ? C14 C13 Cl3 126.9(3) . . ? S1 C13 Cl3 119.3(3) . . ? C13 C14 C15 110.3(4) . . ? C13 C14 C12 125.0(4) . . ? C15 C14 C12 124.7(5) . . ? C16 C15 C14 112.5(5) . . ? C16 C15 H15 123.7 . . ? C14 C15 H15 123.7 . . ? C15 C16 S1 112.6(3) . . ? C15 C16 H16 123.7 . . ? S1 C16 H16 123.7 . . ? C18 C17 C22 117.5(3) . . ? C18 C17 C23 122.3(3) . . ? C22 C17 C23 120.2(3) . . ? C19 C18 C17 121.9(4) . . ? C19 C18 Cl4 118.3(3) . . ? C17 C18 Cl4 119.8(3) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C21 C20 C19 122.2(4) . . ? C21 C20 Cl5 118.8(4) . . ? C19 C20 Cl5 118.9(4) . . ? C20 C21 C22 118.5(4) . . ? C20 C21 H21 120.8 . . ? C22 C21 H21 120.7 . . ? C21 C22 C17 121.6(4) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? O2 C23 C17 112.2(3) . . ? O2 C23 C24 105.4(3) . . ? C17 C23 C24 112.1(2) . . ? O2 C23 H23 109.0 . . ? C17 C23 H23 109.0 . . ? C24 C23 H23 109.0 . . ? N3 C24 C23 108.7(2) . . ? N3 C24 H24A 110.0 . . ? C23 C24 H24A 110.0 . . ? N3 C24 H24B 110.0 . . ? C23 C24 H24B 110.0 . . ? H24A C24 H24B 108.3 . . ? N4 C25 N3 109.1(3) . . ? N4 C25 H25 125.4 . . ? N3 C25 H25 125.4 . . ? C27 C26 N4 106.7(4) . . ? C27 C26 H26 126.6 . . ? N4 C26 H26 126.6 . . ? C26 C27 N3 107.7(4) . . ? C26 C27 H27 126.1 . . ? N3 C27 H27 126.1 . . ? O2 C28 C30B 109.7(4) . . ? O2 C28 C30A 103.3(4) . . ? C30B C28 C30A 17.4(4) . . ? O2 C28 H28A 111(3) . . ? C30B C28 H28A 122(3) . . ? C30A C28 H28A 112(3) . . ? O2 C28 H28B 113(3) . . ? C30B C28 H28B 98(3) . . ? C30A C28 H28B 115(3) . . ? H28A C28 H28B 103(4) . . ? Cl6B C29A C30B 125.0(18) . . ? Cl6B C29A Cl6A 5.0(10) . . ? C30B C29A Cl6A 123.6(15) . . ? Cl6B C29A S2A 121.5(14) . . ? C30B C29A S2A 112.8(14) . . ? Cl6A C29A S2A 123.5(9) . . ? Cl6B C29A C30A 135.4(17) . . ? C30B C29A C30A 10.5(5) . . ? Cl6A C29A C30A 133.8(14) . . ? S2A C29A C30A 102.7(12) . . ? Cl6B C29A S2B 138.8(13) . . ? C30B C29A S2B 95.4(10) . . ? Cl6A C29A S2B 140.9(10) . . ? S2A C29A S2B 17.4(8) . . ? C30A C29A S2B 85.3(9) . . ? C30B C29B C30A 17.0(8) . . ? C30B C29B S2A 144(2) . . ? C30A C29B S2A 126.6(19) . . ? C30B C29B Cl6B 117(2) . . ? C30A C29B Cl6B 134.0(19) . . ? S2A C29B Cl6B 99.2(13) . . ? C30B C29B S2B 123.6(19) . . ? C30A C29B S2B 106.7(15) . . ? S2A C29B S2B 19.9(9) . . ? Cl6B C29B S2B 119.1(12) . . ? C30B C29B C31A 49.3(15) . . ? C30A C29B C31A 32.6(12) . . ? S2A C29B C31A 94.2(14) . . ? Cl6B C29B C31A 166.5(18) . . ? S2B C29B C31A 74.3(13) . . ? C30B C29B Cl6A 115(2) . . ? C30A C29B Cl6A 131.2(17) . . ? S2A C29B Cl6A 101.8(9) . . ? Cl6B C29B Cl6A 4.0(7) . . ? S2B C29B Cl6A 121.6(10) . . ? C31A C29B Cl6A 163.8(15) . . ? C31A C30A C29B 102.5(16) . . ? C31A C30A C31B 13.8(18) . . ? C29B C30A C31B 116.1(16) . . ? C31A C30A C28 145.3(14) . . ? C29B C30A C28 111.4(16) . . ? C31B C30A C28 132.3(18) . . ? C31A C30A C29A 110.4(13) . . ? C29B C30A C29A 8.2(15) . . ? C31B C30A C29A 123.8(14) . . ? C28 C30A C29A 103.8(13) . . ? C29B C30B C29A 14.7(19) . . ? C29B C30B C31A 97.4(19) . . ? C29A C30B C31A 111.7(12) . . ? C29B C30B C28 145.7(19) . . ? C29A C30B C28 131.3(13) . . ? C31A C30B C28 116.9(9) . . ? C29B C30B C31B 105.1(18) . . ? C29A C30B C31B 119.3(13) . . ? C31A C30B C31B 7.9(14) . . ? C28 C30B C31B 109.3(13) . . ? C31B C31A C30A 138(5) . . ? C31B C31A C32B 72(4) . . ? C30A C31A C32B 148(2) . . ? C31B C31A C30B 150(5) . . ? C30A C31A C30B 12.0(7) . . ? C32B C31A C30B 136.6(19) . . ? C31B C31A C32A 97(5) . . ? C30A C31A C32A 123.3(16) . . ? C32B C31A C32A 24.6(17) . . ? C30B C31A C32A 112.0(13) . . ? C31B C31A C29B 173(5) . . ? C30A C31A C29B 44.9(12) . . ? C32B C31A C29B 103(2) . . ? C30B C31A C29B 33.3(10) . . ? C32A C31A C29B 78.8(14) . . ? C31B C31A S2B 124(5) . . ? C30A C31A S2B 96.1(10) . . ? C32B C31A S2B 51.9(14) . . ? C30B C31A S2B 84.7(8) . . ? C32A C31A S2B 27.3(10) . . ? C29B C31A S2B 51.4(11) . . ? C31A C31B C32B 84(5) . . ? C31A C31B C30A 28(3) . . ? C32B C31B C30A 111(2) . . ? C31A C31B C32A 64(5) . . ? C32B C31B C32A 19.4(19) . . ? C30A C31B C32A 91.6(18) . . ? C31A C31B C30B 22(4) . . ? C32B C31B C30B 105(2) . . ? C30A C31B C30B 6.1(6) . . ? C32A C31B C30B 85.8(14) . . ? C32B C32A S2B 176(6) . . ? C32B C32A C31A 60(4) . . ? S2B C32A C31A 116(2) . . ? C32B C32A C31B 42(4) . . ? S2B C32A C31B 135(2) . . ? C31A C32A C31B 18.7(7) . . ? C32B C32A S2A 169(6) . . ? S2B C32A S2A 6.9(9) . . ? C31A C32A S2A 109.2(15) . . ? C31B C32A S2A 127.8(16) . . ? C32A C32B C31B 119(6) . . ? C32A C32B C31A 95(5) . . ? C31B C32B C31A 23.9(13) . . ? C32A C32B S2B 3(4) . . ? C31B C32B S2B 116(2) . . ? C31A C32B S2B 92.8(18) . . ? C9 N1 C11 108.0(4) . . ? C9 N1 C8 125.7(3) . . ? C11 N1 C8 126.3(4) . . ? C9 N2 C10 107.9(4) . . ? C9 N2 H2N 117(4) . . ? C10 N2 H2N 135(4) . . ? C25 N3 C27 107.2(3) . . ? C25 N3 C24 125.9(3) . . ? C27 N3 C24 126.7(3) . . ? C25 N4 C26 109.2(3) . . ? C25 N4 H4N 128(5) . . ? C26 N4 H4N 122(5) . . ? C12 O1 C7 112.2(3) . . ? C23 O2 C28 112.0(3) . . ? H7A O7 H7B 107(7) . . ? H10A O10 H10B 82(4) . . ? H11A O11 H11B 83(4) . . ? C16 S1 C13 90.8(2) . . ? S2B S2A C29B 90.7(17) . . ? S2B S2A C29A 107.0(16) . . ? C29B S2A C29A 16.5(7) . . ? S2B S2A C32A 12.9(15) . . ? C29B S2A C32A 77.8(11) . . ? C29A S2A C32A 94.2(9) . . ? S2A S2B C32A 160(2) . . ? S2A S2B C32B 158.9(19) . . ? C32A S2B C32B 1(2) . . ? S2A S2B C29B 69.4(16) . . ? C32A S2B C29B 90.8(14) . . ? C32B S2B C29B 89.6(11) . . ? S2A S2B C29A 55.6(15) . . ? C32A S2B C29A 104.6(14) . . ? C32B S2B C29A 103.4(10) . . ? C29B S2B C29A 14.0(5) . . ? S2A S2B C31A 123.6(17) . . ? C32A S2B C31A 36.6(13) . . ? C32B S2B C31A 35.4(10) . . ? C29B S2B C31A 54.2(6) . . ? C29A S2B C31A 68.1(5) . . ? O5 S3 O6 110.74(18) . . ? O5 S3 O3 109.16(18) . . ? O6 S3 O3 109.86(17) . . ? O5 S3 O4 109.26(17) . . ? O6 S3 O4 109.18(16) . . ? O3 S3 O4 108.60(18) . . ? C29A Cl6A C29B 5.6(12) . . ? C29A Cl6B C29B 7.1(16) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.380(6) . ? C1 C2 1.388(4) . ? C1 C7 1.523(5) . ? C2 C3 1.388(6) . ? C2 Cl1 1.741(4) . ? C3 C4 1.371(8) . ? C3 H3 0.9300 . ? C4 C5 1.383(7) . ? C4 Cl2 1.736(5) . ? C5 C6 1.385(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 O1 1.423(3) . ? C7 C8 1.517(6) . ? C7 H7 0.9800 . ? C8 N1 1.475(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N1 1.309(6) . ? C9 N2 1.319(6) . ? C9 H9 0.9300 . ? C10 C11 1.325(8) . ? C10 N2 1.350(8) . ? C10 H10 0.9300 . ? C11 N1 1.360(6) . ? C11 H11 0.9300 . ? C12 O1 1.419(5) . ? C12 C14 1.494(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.355(7) . ? C13 S1 1.705(4) . ? C13 Cl3 1.721(5) . ? C14 C15 1.424(6) . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 S1 1.686(6) . ? C16 H16 0.9300 . ? C17 C18 1.385(5) . ? C17 C22 1.395(5) . ? C17 C23 1.525(5) . ? C18 C19 1.383(6) . ? C18 Cl4 1.736(4) . ? C19 C20 1.373(7) . ? C19 H19 0.9300 . ? C20 C21 1.365(7) . ? C20 Cl5 1.754(4) . ? C21 C22 1.384(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 O2 1.421(4) . ? C23 C24 1.534(5) . ? C23 H23 0.9800 . ? C24 N3 1.458(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N4 1.306(5) . ? C25 N3 1.328(5) . ? C25 H25 0.9300 . ? C26 C27 1.332(7) . ? C26 N4 1.368(6) . ? C26 H26 0.9300 . ? C27 N3 1.381(5) . ? C27 H27 0.9300 . ? C28 O2 1.433(4) . ? C28 C30B 1.480(8) . ? C28 C30A 1.559(11) . ? C28 H28A 1.06(5) . ? C28 H28B 1.05(5) . ? C29A Cl6B 1.25(2) . ? C29A C30B 1.397(19) . ? C29A Cl6A 1.663(19) . ? C29A S2A 1.68(2) . ? C29A C30A 1.77(3) . ? C29A S2B 1.95(2) . ? C29B C30B 1.02(3) . ? C29B C30A 1.34(3) . ? C29B S2A 1.67(3) . ? C29B Cl6B 1.69(2) . ? C29B S2B 1.78(3) . ? C29B C31A 1.85(2) . ? C29B Cl6A 2.11(2) . ? C30A C31A 1.02(2) . ? C30A C31B 1.45(3) . ? C30B C31A 1.41(2) . ? C30B C31B 1.88(3) . ? C31A C31B 0.52(2) . ? C31A C32B 1.27(4) . ? C31A C32A 1.46(3) . ? C31A S2B 2.20(2) . ? C31B C32B 1.22(3) . ? C31B C32A 1.60(4) . ? C32A C32B 0.61(3) . ? C32A S2B 1.12(3) . ? C32A S2A 1.71(2) . ? C32B S2B 1.73(3) . ? N2 H2N 0.93(7) . ? N4 H4N 0.87(8) . ? O3 S3 1.473(3) . ? O4 S3 1.491(3) . ? O5 S3 1.461(3) . ? O6 S3 1.466(3) . ? O7 H7A 0.91(7) . ? O7 H7B 0.86(8) . ? O9A O9B 1.01(3) . ? O10 H10A 0.953(18) . ? O10 H10B 0.90(2) . ? O11 H11A 0.90(2) . ? O11 H11B 0.956(18) . ? S2A S2B 0.61(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 -0.5(6) . . . . ? C7 C1 C2 C3 -179.2(4) . . . . ? C6 C1 C2 Cl1 178.3(3) . . . . ? C7 C1 C2 Cl1 -0.5(5) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? Cl1 C2 C3 C4 -177.9(3) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? C2 C3 C4 Cl2 177.8(3) . . . . ? C3 C4 C5 C6 1.3(8) . . . . ? Cl2 C4 C5 C6 -177.8(3) . . . . ? C2 C1 C6 C5 0.5(6) . . . . ? C7 C1 C6 C5 179.2(4) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C6 C1 C7 O1 24.1(5) . . . . ? C2 C1 C7 O1 -157.2(3) . . . . ? C6 C1 C7 C8 -94.4(4) . . . . ? C2 C1 C7 C8 84.3(4) . . . . ? O1 C7 C8 N1 58.8(4) . . . . ? C1 C7 C8 N1 179.6(3) . . . . ? N2 C10 C11 N1 -1.0(7) . . . . ? S1 C13 C14 C15 -0.6(5) . . . . ? Cl3 C13 C14 C15 179.3(3) . . . . ? S1 C13 C14 C12 178.8(3) . . . . ? Cl3 C13 C14 C12 -1.2(7) . . . . ? O1 C12 C14 C13 112.1(5) . . . . ? O1 C12 C14 C15 -68.5(6) . . . . ? C13 C14 C15 C16 0.9(5) . . . . ? C12 C14 C15 C16 -178.5(4) . . . . ? C14 C15 C16 S1 -0.8(5) . . . . ? C22 C17 C18 C19 0.6(5) . . . . ? C23 C17 C18 C19 -177.0(3) . . . . ? C22 C17 C18 Cl4 -179.7(3) . . . . ? C23 C17 C18 Cl4 2.8(4) . . . . ? C17 C18 C19 C20 -0.3(6) . . . . ? Cl4 C18 C19 C20 180.0(3) . . . . ? C18 C19 C20 C21 -0.8(7) . . . . ? C18 C19 C20 Cl5 178.9(3) . . . . ? C19 C20 C21 C22 1.5(7) . . . . ? Cl5 C20 C21 C22 -178.2(4) . . . . ? C20 C21 C22 C17 -1.1(7) . . . . ? C18 C17 C22 C21 0.1(6) . . . . ? C23 C17 C22 C21 177.8(4) . . . . ? C18 C17 C23 O2 162.1(3) . . . . ? C22 C17 C23 O2 -15.4(4) . . . . ? C18 C17 C23 C24 -79.4(4) . . . . ? C22 C17 C23 C24 103.0(4) . . . . ? O2 C23 C24 N3 -62.3(3) . . . . ? C17 C23 C24 N3 175.3(3) . . . . ? N4 C26 C27 N3 0.6(6) . . . . ? C30B C29B C30A C31A 168(3) . . . . ? S2A C29B C30A C31A -8(2) . . . . ? Cl6B C29B C30A C31A 177(2) . . . . ? S2B C29B C30A C31A -6.8(16) . . . . ? Cl6A C29B C30A C31A -178.8(17) . . . . ? C30B C29B C30A C31B 171(3) . . . . ? S2A C29B C30A C31B -5(2) . . . . ? Cl6B C29B C30A C31B 179.9(19) . . . . ? S2B C29B C30A C31B -4.2(18) . . . . ? C31A C29B C30A C31B 2.5(17) . . . . ? Cl6A C29B C30A C31B -176.3(16) . . . . ? C30B C29B C30A C28 -5(2) . . . . ? S2A C29B C30A C28 179.4(13) . . . . ? Cl6B C29B C30A C28 5(3) . . . . ? S2B C29B C30A C28 -179.4(8) . . . . ? C31A C29B C30A C28 -172.6(14) . . . . ? Cl6A C29B C30A C28 9(2) . . . . ? C30B C29B C30A C29A -29(11) . . . . ? S2A C29B C30A C29A 155(13) . . . . ? Cl6B C29B C30A C29A -20(10) . . . . ? S2B C29B C30A C29A 156(13) . . . . ? C31A C29B C30A C29A 163(12) . . . . ? Cl6A C29B C30A C29A -16(10) . . . . ? O2 C28 C30A C31A 82.2(19) . . . . ? C30B C28 C30A C31A -164(3) . . . . ? O2 C28 C30A C29B -110.5(11) . . . . ? C30B C28 C30A C29B 3.2(14) . . . . ? O2 C28 C30A C31B 75.4(13) . . . . ? C30B C28 C30A C31B -171(2) . . . . ? O2 C28 C30A C29A -107.0(8) . . . . ? C30B C28 C30A C29A 6.6(14) . . . . ? Cl6B C29A C30A C31A 170(2) . . . . ? C30B C29A C30A C31A 163(3) . . . . ? Cl6A C29A C30A C31A 176.6(17) . . . . ? S2A C29A C30A C31A -2.5(16) . . . . ? S2B C29A C30A C31A -3.1(13) . . . . ? Cl6B C29A C30A C29B 152(14) . . . . ? C30B C29A C30A C29B 145(13) . . . . ? Cl6A C29A C30A C29B 159(13) . . . . ? S2A C29A C30A C29B -20(11) . . . . ? S2B C29A C30A C29B -21(11) . . . . ? Cl6B C29A C30A C31B 173(2) . . . . ? C30B C29A C30A C31B 166(3) . . . . ? Cl6A C29A C30A C31B -179.9(16) . . . . ? S2A C29A C30A C31B 1.0(17) . . . . ? S2B C29A C30A C31B 0.4(15) . . . . ? Cl6B C29A C30A C28 -4(2) . . . . ? C30B C29A C30A C28 -12(2) . . . . ? Cl6A C29A C30A C28 2.2(19) . . . . ? S2A C29A C30A C28 -176.9(9) . . . . ? S2B C29A C30A C28 -177.5(6) . . . . ? C30A C29B C30B C29A 160(8) . . . . ? S2A C29B C30B C29A 165(11) . . . . ? Cl6B C29B C30B C29A -13(7) . . . . ? S2B C29B C30B C29A 166(10) . . . . ? C31A C29B C30B C29A 168(8) . . . . ? Cl6A C29B C30B C29A -9(7) . . . . ? C30A C29B C30B C31A -8.5(19) . . . . ? S2A C29B C30B C31A -3(3) . . . . ? Cl6B C29B C30B C31A 179.1(16) . . . . ? S2B C29B C30B C31A -2.5(19) . . . . ? Cl6A C29B C30B C31A -177.6(13) . . . . ? C30A C29B C30B C28 172(4) . . . . ? S2A C29B C30B C28 177.4(14) . . . . ? Cl6B C29B C30B C28 -1(3) . . . . ? S2B C29B C30B C28 177.9(8) . . . . ? C31A C29B C30B C28 -180(2) . . . . ? Cl6A C29B C30B C28 3(3) . . . . ? C30A C29B C30B C31B -6.8(18) . . . . ? S2A C29B C30B C31B -1(3) . . . . ? Cl6B C29B C30B C31B -179.2(14) . . . . ? S2B C29B C30B C31B -1(2) . . . . ? C31A C29B C30B C31B 1.7(12) . . . . ? Cl6A C29B C30B C31B -175.9(12) . . . . ? Cl6B C29A C30B C29B 161(10) . . . . ? Cl6A C29A C30B C29B 167(9) . . . . ? S2A C29A C30B C29B -9(7) . . . . ? C30A C29A C30B C29B -25(9) . . . . ? S2B C29A C30B C29B -11(8) . . . . ? Cl6B C29A C30B C31A 173.7(17) . . . . ? Cl6A C29A C30B C31A 179.5(13) . . . . ? S2A C29A C30B C31A 3.2(17) . . . . ? C30A C29A C30B C31A -12(2) . . . . ? S2B C29A C30B C31A 1.7(13) . . . . ? Cl6B C29A C30B C28 -10(3) . . . . ? Cl6A C29A C30B C28 -4(2) . . . . ? S2A C29A C30B C28 179.7(7) . . . . ? C30A C29A C30B C28 164(3) . . . . ? S2B C29A C30B C28 178.2(6) . . . . ? Cl6B C29A C30B C31B 176.1(16) . . . . ? Cl6A C29A C30B C31B -178.1(12) . . . . ? S2A C29A C30B C31B 5.6(18) . . . . ? C30A C29A C30B C31B -10(2) . . . . ? S2B C29A C30B C31B 4.1(14) . . . . ? O2 C28 C30B C29B -102(2) . . . . ? C30A C28 C30B C29B -173(3) . . . . ? O2 C28 C30B C29A -97.9(13) . . . . ? C30A C28 C30B C29A -169(2) . . . . ? O2 C28 C30B C31A 78.4(8) . . . . ? C30A C28 C30B C31A 7.2(13) . . . . ? O2 C28 C30B C31B 76.6(8) . . . . ? C30A C28 C30B C31B 5.4(14) . . . . ? C29B C30A C31A C31B 170(6) . . . . ? C28 C30A C31A C31B -22(8) . . . . ? C29A C30A C31A C31B 168(6) . . . . ? C29B C30A C31A C32B 12(4) . . . . ? C31B C30A C31A C32B -158(9) . . . . ? C28 C30A C31A C32B -180(3) . . . . ? C29A C30A C31A C32B 10(4) . . . . ? C29B C30A C31A C30B -12(3) . . . . ? C31B C30A C31A C30B 177(6) . . . . ? C28 C30A C31A C30B 156(4) . . . . ? C29A C30A C31A C30B -15(3) . . . . ? C29B C30A C31A C32A 8(2) . . . . ? C31B C30A C31A C32A -162(8) . . . . ? C28 C30A C31A C32A 176.3(14) . . . . ? C29A C30A C31A C32A 6(2) . . . . ? C31B C30A C31A C29B -170(6) . . . . ? C28 C30A C31A C29B 168(2) . . . . ? C29A C30A C31A C29B -2.6(16) . . . . ? C29B C30A C31A S2B 5.3(13) . . . . ? C31B C30A C31A S2B -165(7) . . . . ? C28 C30A C31A S2B 173.2(14) . . . . ? C29A C30A C31A S2B 2.8(12) . . . . ? C29B C30B C31A C31B 168(9) . . . . ? C29A C30B C31A C31B 164(8) . . . . ? C28 C30B C31A C31B -13(9) . . . . ? C29B C30B C31A C30A 164(3) . . . . ? C29A C30B C31A C30A 161(3) . . . . ? C28 C30B C31A C30A -16(3) . . . . ? C31B C30B C31A C30A -4(8) . . . . ? C29B C30B C31A C32B 3(3) . . . . ? C29A C30B C31A C32B 0(3) . . . . ? C28 C30B C31A C32B -177(2) . . . . ? C31B C30B C31A C32B -165(10) . . . . ? C29B C30B C31A C32A 2.7(18) . . . . ? C29A C30B C31A C32A -0.5(17) . . . . ? C28 C30B C31A C32A -177.6(11) . . . . ? C31B C30B C31A C32A -165(9) . . . . ? C29A C30B C31A C29B -3(2) . . . . ? C28 C30B C31A C29B 179.8(15) . . . . ? C31B C30B C31A C29B -168(9) . . . . ? C29B C30B C31A S2B 1.7(13) . . . . ? C29A C30B C31A S2B -1.5(11) . . . . ? C28 C30B C31A S2B -178.6(5) . . . . ? C31B C30B C31A S2B -166(9) . . . . ? C30B C29B C31A C30A -4.6(10) . . . . ? S2A C29B C31A C30A 173.6(18) . . . . ? Cl6B C29B C31A C30A -8(6) . . . . ? S2B C29B C31A C30A 173.2(16) . . . . ? Cl6A C29B C31A C30A 3(5) . . . . ? C30B C29B C31A C32B -178(2) . . . . ? C30A C29B C31A C32B -173(2) . . . . ? S2A C29B C31A C32B 0.2(19) . . . . ? Cl6B C29B C31A C32B 179(6) . . . . ? S2B C29B C31A C32B -0.1(16) . . . . ? Cl6A C29B C31A C32B -170(5) . . . . ? C30A C29B C31A C30B 4.6(10) . . . . ? S2A C29B C31A C30B 178.2(19) . . . . ? Cl6B C29B C31A C30B -3(6) . . . . ? S2B C29B C31A C30B 177.9(17) . . . . ? Cl6A C29B C31A C30B 8(4) . . . . ? C30B C29B C31A C32A -177.5(17) . . . . ? C30A C29B C31A C32A -172.9(18) . . . . ? S2A C29B C31A C32A 0.7(13) . . . . ? Cl6B C29B C31A C32A 179(7) . . . . ? S2B C29B C31A C32A 0.4(11) . . . . ? Cl6A C29B C31A C32A -170(5) . . . . ? C30B C29B C31A S2B -177.9(17) . . . . ? C30A C29B C31A S2B -173.2(16) . . . . ? S2A C29B C31A S2B 0.3(7) . . . . ? Cl6B C29B C31A S2B 179(7) . . . . ? Cl6A C29B C31A S2B -170(5) . . . . ? C30A C31A C31B C32B -168(5) . . . . ? C30B C31A C31B C32B -169(7) . . . . ? C32A C31A C31B C32B -3(3) . . . . ? S2B C31A C31B C32B -6(4) . . . . ? C32B C31A C31B C30A 168(5) . . . . ? C30B C31A C31B C30A -1(2) . . . . ? C32A C31A C31B C30A 165(7) . . . . ? S2B C31A C31B C30A 162(8) . . . . ? C30A C31A C31B C32A -165(7) . . . . ? C32B C31A C31B C32A 3(3) . . . . ? C30B C31A C31B C32A -166(9) . . . . ? S2B C31A C31B C32A -3(2) . . . . ? C30A C31A C31B C30B 1(2) . . . . ? C32B C31A C31B C30B 169(7) . . . . ? C32A C31A C31B C30B 166(9) . . . . ? S2B C31A C31B C30B 163(10) . . . . ? C29B C30A C31B C31A -10(7) . . . . ? C28 C30A C31B C31A 163(6) . . . . ? C29A C30A C31B C31A -14(7) . . . . ? C31A C30A C31B C32B 13(6) . . . . ? C29B C30A C31B C32B 2(3) . . . . ? C28 C30A C31B C32B 176.2(17) . . . . ? C29A C30A C31B C32B -1(3) . . . . ? C31A C30A C31B C32A 14(6) . . . . ? C29B C30A C31B C32A 3.1(18) . . . . ? C28 C30A C31B C32A 177.0(10) . . . . ? C29A C30A C31B C32A -0.2(18) . . . . ? C31A C30A C31B C30B -4(9) . . . . ? C29B C30A C31B C30B -14(4) . . . . ? C28 C30A C31B C30B 159(5) . . . . ? C29A C30A C31B C30B -18(4) . . . . ? C29B C30B C31B C31A -13(9) . . . . ? C29A C30B C31B C31A -17(9) . . . . ? C28 C30B C31B C31A 168(8) . . . . ? C29B C30B C31B C32B -1(2) . . . . ? C29A C30B C31B C32B -5(2) . . . . ? C31A C30B C31B C32B 11(8) . . . . ? C28 C30B C31B C32B 179.4(17) . . . . ? C29B C30B C31B C30A 162(5) . . . . ? C29A C30B C31B C30A 158(5) . . . . ? C31A C30B C31B C30A 175(11) . . . . ? C28 C30B C31B C30A -17(4) . . . . ? C29B C30B C31B C32A 0.0(17) . . . . ? C29A C30B C31B C32A -3.9(16) . . . . ? C31A C30B C31B C32A 13(8) . . . . ? C28 C30B C31B C32A -179.2(10) . . . . ? C31B C31A C32A C32B 7(6) . . . . ? C30A C31A C32A C32B 175(5) . . . . ? C30B C31A C32A C32B 180(5) . . . . ? C29B C31A C32A C32B -179(5) . . . . ? S2B C31A C32A C32B -178(6) . . . . ? C31B C31A C32A S2B -175(4) . . . . ? C30A C31A C32A S2B -7(3) . . . . ? C32B C31A C32A S2B 178(6) . . . . ? C30B C31A C32A S2B -2(2) . . . . ? C29B C31A C32A S2B -0.7(18) . . . . ? C30A C31A C32A C31B 168(5) . . . . ? C32B C31A C32A C31B -7(6) . . . . ? C30B C31A C32A C31B 173(4) . . . . ? C29B C31A C32A C31B 174(4) . . . . ? S2B C31A C32A C31B 175(4) . . . . ? C31B C31A C32A S2A -175(4) . . . . ? C30A C31A C32A S2A -7(2) . . . . ? C32B C31A C32A S2A 178(6) . . . . ? C30B C31A C32A S2A -2.2(18) . . . . ? C29B C31A C32A S2A -0.8(13) . . . . ? S2B C31A C32A S2A -0.1(10) . . . . ? C31A C31B C32A C32B -171(8) . . . . ? C30A C31B C32A C32B -178(6) . . . . ? C30B C31B C32A C32B -176(6) . . . . ? C31A C31B C32A S2B 7(5) . . . . ? C32B C31B C32A S2B 177(8) . . . . ? C30A C31B C32A S2B 0(3) . . . . ? C30B C31B C32A S2B 1(3) . . . . ? C32B C31B C32A C31A 171(8) . . . . ? C30A C31B C32A C31A -7(3) . . . . ? C30B C31B C32A C31A -5(3) . . . . ? C31A C31B C32A S2A 6(4) . . . . ? C32B C31B C32A S2A 177(7) . . . . ? C30A C31B C32A S2A -1(2) . . . . ? C30B C31B C32A S2A 1.0(19) . . . . ? C31A C32A C32B C31B -3(3) . . . . ? S2A C32A C32B C31B -13(31) . . . . ? C31B C32A C32B C31A 3(3) . . . . ? S2A C32A C32B C31A -10(29) . . . . ? C31A C32A C32B S2B 24(83) . . . . ? C31B C32A C32B S2B 28(85) . . . . ? S2A C32A C32B S2B 15(56) . . . . ? C31A C31B C32B C32A 8(7) . . . . ? C30A C31B C32B C32A 2(7) . . . . ? C30B C31B C32B C32A 4(6) . . . . ? C30A C31B C32B C31A -6(3) . . . . ? C32A C31B C32B C31A -8(7) . . . . ? C30B C31B C32B C31A -4(3) . . . . ? C31A C31B C32B S2B 7(4) . . . . ? C30A C31B C32B S2B 1(3) . . . . ? C32A C31B C32B S2B -1(4) . . . . ? C30B C31B C32B S2B 3(2) . . . . ? C31B C31A C32B C32A -173(6) . . . . ? C30A C31A C32B C32A -8(7) . . . . ? C30B C31A C32B C32A 0(6) . . . . ? C29B C31A C32B C32A 1(5) . . . . ? S2B C31A C32B C32A 1(4) . . . . ? C30A C31A C32B C31B 165(6) . . . . ? C30B C31A C32B C31B 172(5) . . . . ? C32A C31A C32B C31B 173(6) . . . . ? C29B C31A C32B C31B 174(4) . . . . ? S2B C31A C32B C31B 174(4) . . . . ? C31B C31A C32B S2B -174(4) . . . . ? C30A C31A C32B S2B -9(4) . . . . ? C30B C31A C32B S2B -2(3) . . . . ? C32A C31A C32B S2B -1(4) . . . . ? C29B C31A C32B S2B 0.1(16) . . . . ? N2 C9 N1 C11 0.0(6) . . . . ? N2 C9 N1 C8 -179.0(4) . . . . ? C10 C11 N1 C9 0.6(7) . . . . ? C10 C11 N1 C8 179.7(4) . . . . ? C7 C8 N1 C9 -133.5(4) . . . . ? C7 C8 N1 C11 47.7(6) . . . . ? N1 C9 N2 C10 -0.6(6) . . . . ? C11 C10 N2 C9 1.0(7) . . . . ? N4 C25 N3 C27 -0.2(4) . . . . ? N4 C25 N3 C24 175.8(3) . . . . ? C26 C27 N3 C25 -0.3(6) . . . . ? C26 C27 N3 C24 -176.2(4) . . . . ? C23 C24 N3 C25 -84.3(4) . . . . ? C23 C24 N3 C27 90.8(5) . . . . ? N3 C25 N4 C26 0.6(5) . . . . ? C27 C26 N4 C25 -0.8(6) . . . . ? C14 C12 O1 C7 176.6(4) . . . . ? C8 C7 O1 C12 -158.9(4) . . . . ? C1 C7 O1 C12 81.9(4) . . . . ? C17 C23 O2 C28 -86.7(4) . . . . ? C24 C23 O2 C28 151.0(3) . . . . ? C30B C28 O2 C23 168.7(5) . . . . ? C30A C28 O2 C23 -174.4(6) . . . . ? C15 C16 S1 C13 0.4(4) . . . . ? C14 C13 S1 C16 0.2(4) . . . . ? Cl3 C13 S1 C16 -179.8(3) . . . . ? C30B C29B S2A S2B 1(4) . . . . ? C30A C29B S2A S2B 3(3) . . . . ? Cl6B C29B S2A S2B 179.4(19) . . . . ? C31A C29B S2A S2B -1.0(19) . . . . ? Cl6A C29B S2A S2B 176.3(18) . . . . ? C30B C29B S2A C29A -169(8) . . . . ? C30A C29B S2A C29A -167(6) . . . . ? Cl6B C29B S2A C29A 9(4) . . . . ? S2B C29B S2A C29A -170(5) . . . . ? C31A C29B S2A C29A -171(6) . . . . ? Cl6A C29B S2A C29A 6(4) . . . . ? C30B C29B S2A C32A 2(3) . . . . ? C30A C29B S2A C32A 3.7(18) . . . . ? Cl6B C29B S2A C32A 179.8(14) . . . . ? S2B C29B S2A C32A 0.3(16) . . . . ? C31A C29B S2A C32A -0.6(11) . . . . ? Cl6A C29B S2A C32A 176.7(13) . . . . ? Cl6B C29A S2A S2B -176(2) . . . . ? C30B C29A S2A S2B -5(2) . . . . ? Cl6A C29A S2A S2B 179(2) . . . . ? C30A C29A S2A S2B -2(2) . . . . ? Cl6B C29A S2A C29B -166(6) . . . . ? C30B C29A S2A C29B 5(4) . . . . ? Cl6A C29A S2A C29B -171(6) . . . . ? C30A C29A S2A C29B 8(4) . . . . ? S2B C29A S2A C29B 10(5) . . . . ? Cl6B C29A S2A C32A -174.8(19) . . . . ? C30B C29A S2A C32A -3.9(16) . . . . ? Cl6A C29A S2A C32A 179.7(15) . . . . ? C30A C29A S2A C32A -1.0(13) . . . . ? S2B C29A S2A C32A 1.0(17) . . . . ? C32B C32A S2A S2B -172(31) . . . . ? C31A C32A S2A S2B 179(7) . . . . ? C31B C32A S2A S2B 177(8) . . . . ? C32B C32A S2A C29B 10(27) . . . . ? S2B C32A S2A C29B -178(7) . . . . ? C31A C32A S2A C29B 0.8(14) . . . . ? C31B C32A S2A C29B -1.3(19) . . . . ? C32B C32A S2A C29A 12(28) . . . . ? S2B C32A S2A C29A -176(7) . . . . ? C31A C32A S2A C29A 3.5(16) . . . . ? C31B C32A S2A C29A 1(2) . . . . ? C29B S2A S2B C32A 2(7) . . . . ? C29A S2A S2B C32A 4(7) . . . . ? C29B S2A S2B C32B 3(5) . . . . ? C29A S2A S2B C32B 6(6) . . . . ? C32A S2A S2B C32B 1(6) . . . . ? C29A S2A S2B C29B 2.8(15) . . . . ? C32A S2A S2B C29B -2(7) . . . . ? C29B S2A S2B C29A -2.8(15) . . . . ? C32A S2A S2B C29A -4(7) . . . . ? C29B S2A S2B C31A 1.0(19) . . . . ? C29A S2A S2B C31A 4(2) . . . . ? C32A S2A S2B C31A -1(6) . . . . ? C31A C32A S2B S2A -1(8) . . . . ? C31B C32A S2B S2A -3(8) . . . . ? C31A C32A S2B C32B -23(80) . . . . ? C31B C32A S2B C32B -26(79) . . . . ? S2A C32A S2B C32B -23(85) . . . . ? C31A C32A S2B C29B 0.7(18) . . . . ? C31B C32A S2B C29B -2(3) . . . . ? S2A C32A S2B C29B 1(7) . . . . ? C31A C32A S2B C29A 3(2) . . . . ? C31B C32A S2B C29A 1(3) . . . . ? S2A C32A S2B C29A 4(6) . . . . ? C31B C32A S2B C31A -2.4(17) . . . . ? S2A C32A S2B C31A 1(8) . . . . ? C32A C32B S2B S2A -159(80) . . . . ? C31B C32B S2B S2A -6(6) . . . . ? C31A C32B S2B S2A -3(6) . . . . ? C31B C32B S2B C32A 153(83) . . . . ? C31A C32B S2B C32A 156(82) . . . . ? C32A C32B S2B C29B -156(81) . . . . ? C31B C32B S2B C29B -3(2) . . . . ? C31A C32B S2B C29B -0.1(16) . . . . ? C32A C32B S2B C29A -154(81) . . . . ? C31B C32B S2B C29A -1(2) . . . . ? C31A C32B S2B C29A 2.0(18) . . . . ? C32A C32B S2B C31A -156(82) . . . . ? C31B C32B S2B C31A -2.9(17) . . . . ? C30B C29B S2B S2A -179(3) . . . . ? C30A C29B S2B S2A -177(2) . . . . ? Cl6B C29B S2B S2A -1(2) . . . . ? C31A C29B S2B S2A 179(2) . . . . ? Cl6A C29B S2B S2A -4(2) . . . . ? C30B C29B S2B C32A 1(2) . . . . ? C30A C29B S2B C32A 3.3(17) . . . . ? S2A C29B S2B C32A -179(2) . . . . ? Cl6B C29B S2B C32A 179.9(18) . . . . ? C31A C29B S2B C32A -0.5(14) . . . . ? Cl6A C29B S2B C32A 176.3(16) . . . . ? C30B C29B S2B C32B 2(2) . . . . ? C30A C29B S2B C32B 3.9(15) . . . . ? S2A C29B S2B C32B -179(2) . . . . ? Cl6B C29B S2B C32B -179.6(17) . . . . ? C31A C29B S2B C32B 0.1(12) . . . . ? Cl6A C29B S2B C32B 176.8(15) . . . . ? C30B C29B S2B C29A -169(7) . . . . ? C30A C29B S2B C29A -168(6) . . . . ? S2A C29B S2B C29A 10(5) . . . . ? Cl6B C29B S2B C29A 9(4) . . . . ? C31A C29B S2B C29A -171(6) . . . . ? Cl6A C29B S2B C29A 5(4) . . . . ? C30B C29B S2B C31A 1.9(15) . . . . ? C30A C29B S2B C31A 3.8(9) . . . . ? S2A C29B S2B C31A -179(2) . . . . ? Cl6B C29B S2B C31A -179.6(19) . . . . ? Cl6A C29B S2B C31A 176.8(18) . . . . ? Cl6B C29A Cl6A C29B 91(17) . . . . ? C30B C29A Cl6A C29B -16(11) . . . . ? S2A C29A Cl6A C29B 159(13) . . . . ? C30A C29A Cl6A C29B -19(11) . . . . ? S2B C29A Cl6A C29B 160(14) . . . . ? C30B C29A Cl6B C29B -24(10) . . . . ? Cl6A C29A Cl6B C29B -99(17) . . . . ? S2A C29A Cl6B C29B 146(13) . . . . ? C30A C29A Cl6B C29B -25(10) . . . . ? S2B C29A Cl6B C29B 144(13) . . . . ? C30B C29B Cl6B C29A 150(13) . . . . ? C30A C29B Cl6B C29A 147(13) . . . . ? S2A C29B Cl6B C29A -29(11) . . . . ? S2B C29B Cl6B C29A -29(11) . . . . ? C31A C29B Cl6B C29A 153(17) . . . . ? Cl6A C29B Cl6B C29A 101(17) . . . . ?