#------------------------------------------------------------------------------ #$Date: 2024-12-07 17:43:15 +0100 (Sat, 07 Dec 2024) $ #$Revision: 296745 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/33/2023329.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2023329 loop_ _publ_author_name 'Madhan, S.' 'NizamMohideen, M.' 'Pavunkumar, Vinayagam' 'MohanaKrishnan, Arasambattu K.' _publ_section_title ; The crystal structures determination and Hirshfeld surface analysis of N-(4-bromo-3-methoxyphenyl)- and N-{[3-bromo-1-(phenylsulfonyl)-1H-indol-2-yl]methyl}- derivatives of N-{[3-bromo-1-(phenylsulfonyl)-1H-indol-2-yl]methyl}benzenesulfonamide ; _journal_coeditor_code NU2007 _journal_issue 11 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_page_first 1110 _journal_page_last 1117 _journal_paper_doi 10.1107/S2056989024009587 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C36 H27 Br2 N3 O6 S3' _chemical_formula_moiety 'C36 H27 Br2 N3 O6 S3' _chemical_formula_sum 'C36 H27 Br2 N3 O6 S3' _chemical_formula_weight 853.60 _chemical_name_systematic N,N-Bis{[3-bromo-1-(phenylsulfonyl)-1H-indol-2-yl]methyl}benzenesulfonamide _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 90 _cell_angle_beta 104.550(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.2664(4) _cell_length_b 34.7886(18) _cell_length_c 12.5972(6) _cell_measurement_reflns_used 73921 _cell_measurement_temperature 303(2) _cell_measurement_theta_max 24.995 _cell_measurement_theta_min 1.405 _cell_volume 3506.5(3) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX2 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and Mercury (Macrae et al., 2020) ; _computing_publication_material ; WinGX (Farrugia, 2012), pubCIF (Westrip, 2010) and PLATON (Spek, 2020) ; _computing_structure_refinement ; SHELXL2019/2 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 303(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 Venture Diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 73921 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.453 _diffrn_reflns_theta_min 2.671 _diffrn_source 'micro focus sealed tube' _exptl_absorpt_coefficient_mu 2.542 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.4912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.617 _exptl_crystal_description Block _exptl_crystal_F_000 1720 _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.458 _refine_diff_density_min -0.466 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 6434 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0478 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+5.0983P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1133 _refine_ls_wR_factor_ref 0.1199 _reflns_number_gt 5196 _reflns_number_total 6434 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file nu2007.cif _cod_data_source_block II _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2023329 _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 0.526 _shelx_estimated_absorpt_t_max 0.905 _shelx_hkl_file ; -1 0 0 0.90 0.50 -1 0 0 -0.90 0.30 2 0 0 3554.54 267.27 2 0 0 3735.03 267.27 2 0 0 3581.84 267.27 -2 0 0 3566.94 267.17 -2 0 0 3471.55 267.47 -2 0 0 3592.54 267.37 -2 0 0 3348.66 267.27 3 0 0 2.20 1.80 -3 0 0 0.10 1.20 3 0 0 3.50 1.60 3 0 0 -1.70 1.80 3 0 0 2.00 1.60 -3 0 0 0.60 1.50 -3 0 0 -3.80 1.80 -3 0 0 -2.40 2.10 -3 0 0 1.40 2.40 -4 0 0 36.60 4.20 -4 0 0 48.30 6.10 -4 0 0 43.60 4.80 4 0 0 42.80 4.60 4 0 0 44.20 4.50 4 0 0 47.00 4.70 4 0 0 46.50 4.20 -4 0 0 33.60 4.10 5 0 0 -0.20 2.50 -5 0 0 -3.20 3.10 -5 0 0 -0.70 3.50 -5 0 0 1.40 3.80 -5 0 0 3.80 2.30 -5 0 0 4.70 2.10 5 0 0 -4.20 2.80 5 0 0 1.90 2.90 -6 0 0 38.10 4.00 -6 0 0 30.40 5.20 -6 0 0 37.40 6.30 -6 0 0 35.80 4.60 6 0 0 35.20 4.90 6 0 0 30.10 5.00 6 0 0 41.20 4.90 -6 0 0 37.40 5.80 7 0 0 4.50 3.40 7 0 0 -9.30 3.10 -7 0 0 2.40 5.70 -7 0 0 0.80 4.30 -7 0 0 5.90 5.00 7 0 0 3.70 1.70 -8 0 0 7.20 5.50 -8 0 0 22.90 6.30 8 0 0 19.10 5.30 -9 0 0 2.30 6.10 9 0 0 1.20 4.00 -9 0 0 10.10 6.60 -2 -1 0 2283.77 169.98 2 -1 0 2264.87 169.88 -2 -1 0 2293.57 169.88 2 -1 0 2419.06 169.88 2 -1 0 2234.68 169.78 -2 -1 0 2085.29 169.98 -2 -1 0 2128.09 169.78 2 1 0 2435.36 169.78 -2 1 0 2122.79 169.68 2 1 0 2310.67 169.88 -2 1 0 2216.58 169.88 -2 1 0 2092.99 170.08 -2 1 0 2220.38 169.88 -2 1 0 2441.06 170.18 2 1 0 2279.47 169.88 3 -1 0 1.30 1.80 3 -1 0 4.00 1.50 3 -1 0 3.10 1.90 -3 -1 0 2.00 1.50 -3 -1 0 3.40 1.40 -3 -1 0 -0.80 2.00 3 -1 0 5.10 1.80 -3 -1 0 0.20 1.90 -3 1 0 5.40 2.20 -3 1 0 2.40 1.70 -3 1 0 5.20 1.20 3 1 0 6.40 1.60 -3 1 0 10.30 2.80 3 1 0 6.30 1.90 3 1 0 2.70 2.00 3 1 0 3.80 1.90 -3 1 0 7.70 2.00 -4 -1 0 2.90 1.90 4 -1 0 1.40 2.30 4 -1 0 4.80 2.10 4 -1 0 0.20 2.20 -4 -1 0 3.90 1.80 -4 -1 0 0.80 2.60 4 -1 0 5.30 1.70 -4 -1 0 2.10 3.70 -4 1 0 5.70 5.00 -4 1 0 1.50 1.60 4 1 0 7.20 2.10 -4 1 0 0.60 2.50 4 1 0 3.40 2.50 4 1 0 10.20 2.10 4 1 0 4.10 2.50 -4 1 0 6.20 2.10 -5 -1 0 22.40 4.20 -5 -1 0 25.60 4.00 5 -1 0 14.50 3.40 -5 -1 0 20.50 2.90 5 -1 0 10.70 3.10 -5 1 0 14.40 2.40 -5 1 0 7.40 3.70 5 1 0 24.60 3.20 -5 1 0 9.90 4.10 -5 1 0 8.50 2.90 -5 1 0 17.20 4.40 5 1 0 21.00 3.80 -6 -1 0 10.50 4.80 -6 -1 0 10.50 2.90 6 -1 0 3.50 3.40 6 -1 0 9.70 3.40 -6 -1 0 8.00 3.70 6 -1 0 9.50 3.40 -6 -1 0 8.10 4.40 -6 -1 0 3.30 2.40 6 1 0 7.70 3.10 6 1 0 5.40 3.60 -6 1 0 9.30 5.00 -6 1 0 7.80 3.30 -6 1 0 3.50 3.70 6 1 0 1.40 3.10 -6 1 0 0.90 4.40 -7 -1 0 12.70 4.50 7 -1 0 6.10 4.30 -7 -1 0 14.30 2.70 -7 -1 0 9.70 5.10 -7 -1 0 13.70 6.40 7 -1 0 4.50 1.80 -7 1 0 15.80 6.50 7 1 0 5.00 3.70 -7 1 0 9.60 4.60 -7 1 0 6.50 5.10 7 1 0 3.00 1.90 7 1 0 11.10 3.60 -7 1 0 7.40 3.70 -8 -1 0 35.70 7.00 8 -1 0 34.60 5.40 -8 -1 0 32.30 6.70 -8 1 0 28.00 6.60 8 1 0 26.60 4.70 -8 1 0 29.20 6.80 -9 -1 0 12.40 6.80 9 -1 0 18.30 4.80 -9 -1 0 19.20 6.60 -9 1 0 14.90 6.70 -9 1 0 9.80 6.40 -1 -2 0 2.80 0.70 -1 -2 0 0.90 0.60 1 2 0 0.50 0.80 -1 2 0 4.10 0.70 1 2 0 0.90 0.60 2 -2 0 2.50 1.70 -2 -2 0 9.60 1.90 2 -2 0 9.80 1.70 -2 -2 0 9.70 1.30 -2 2 0 2.80 2.00 -2 2 0 9.60 1.60 2 2 0 8.80 2.00 -2 2 0 8.70 2.10 2 2 0 9.80 1.30 -2 2 0 3.70 1.90 3 -2 0 180.48 15.00 -3 -2 0 189.28 15.10 -3 -2 0 174.38 14.70 3 -2 0 186.08 15.00 -3 -2 0 209.18 15.00 -3 -2 0 201.38 15.10 3 2 0 207.28 14.80 -3 2 0 165.28 15.00 3 2 0 203.88 15.10 -3 2 0 210.58 15.50 -3 2 0 182.38 15.10 3 2 0 201.48 15.10 3 2 0 196.18 15.10 -3 2 0 170.58 15.00 -4 -2 0 4.70 1.70 4 -2 0 4.90 2.40 -4 -2 0 3.50 5.30 4 -2 0 6.60 2.30 -4 -2 0 5.60 2.30 -4 -2 0 6.30 2.60 4 -2 0 7.10 2.50 -4 2 0 -0.60 2.60 4 2 0 5.20 2.50 4 2 0 10.50 2.10 -4 2 0 8.20 2.30 4 2 0 9.80 2.60 4 2 0 7.10 2.40 5 -2 0 425.36 34.20 -5 -2 0 454.45 34.40 -5 -2 0 489.65 34.60 5 -2 0 406.76 34.10 -5 -2 0 437.46 33.90 -5 -2 0 482.85 35.20 5 2 0 445.46 34.00 5 2 0 461.15 34.30 -5 2 0 391.66 34.00 -5 2 0 399.36 34.30 -5 2 0 468.25 35.00 5 2 0 432.56 34.10 5 2 0 456.35 33.90 -5 2 0 450.35 34.50 -6 -2 0 197.68 16.30 -6 -2 0 175.58 17.10 6 -2 0 197.88 16.70 -6 -2 0 239.88 17.70 6 -2 0 208.18 17.00 6 2 0 199.28 17.00 -6 2 0 246.08 18.50 -6 2 0 225.08 17.40 6 2 0 205.18 16.50 -6 2 0 198.88 16.70 6 2 0 182.38 16.70 -6 2 0 199.68 17.20 7 -2 0 189.98 16.10 -7 -2 0 192.88 15.10 -7 -2 0 217.28 18.50 -7 -2 0 175.18 16.40 -7 -2 0 225.28 17.10 -7 2 0 201.88 17.00 -7 2 0 173.38 16.40 -7 2 0 176.78 16.40 7 2 0 166.18 15.50 7 2 0 171.48 15.90 8 -2 0 4.50 3.80 -8 -2 0 1.60 5.20 -8 -2 0 6.20 5.70 -8 2 0 1.30 5.20 8 2 0 2.60 3.40 -8 2 0 2.50 5.40 9 -2 0 69.69 10.10 -9 -2 0 90.79 10.50 -9 -2 0 77.99 10.70 9 -2 0 94.19 10.00 -9 2 0 92.59 10.50 9 2 0 89.59 8.70 -9 2 0 81.49 10.80 1 -3 0 0.10 0.50 -1 -3 0 1.90 0.80 1 -3 0 0.30 0.50 1 -3 0 -0.10 0.60 -1 -3 0 0.30 0.70 -1 -3 0 1.80 0.80 1 3 0 -0.10 0.60 1 3 0 0.20 0.80 -1 3 0 3.50 0.90 -1 3 0 2.30 0.80 -1 3 0 6.90 1.20 -2 -3 0 2455.15 193.78 -2 -3 0 2607.34 193.78 2 -3 0 2710.33 193.78 2 -3 0 2507.45 193.68 2 -3 0 2674.13 193.88 -2 -3 0 2744.83 193.78 2 3 0 2642.64 193.78 -2 3 0 2405.16 193.78 -2 3 0 2692.73 193.88 2 3 0 2540.25 193.68 2 3 0 2593.94 193.48 2 3 0 2510.55 193.78 -2 3 0 2388.16 193.68 -2 3 0 2525.95 193.68 -3 -3 0 14.00 2.40 3 -3 0 18.50 2.60 -3 -3 0 11.20 2.50 3 -3 0 17.40 2.50 -3 -3 0 10.20 2.50 3 -3 0 12.80 2.40 -3 3 0 12.50 2.40 3 3 0 9.60 2.40 -3 3 0 18.80 3.00 3 3 0 14.80 1.80 -3 3 0 15.00 2.50 3 3 0 12.60 2.60 3 3 0 8.40 2.40 -3 3 0 14.60 2.70 4 -3 0 10.70 2.70 -4 -3 0 15.10 3.10 4 -3 0 11.30 2.80 4 -3 0 7.80 2.70 -4 3 0 17.40 3.10 -4 3 0 16.50 5.40 4 3 0 18.10 3.10 -4 3 0 14.50 2.80 4 3 0 22.40 3.20 -5 -3 0 124.99 11.10 -5 -3 0 135.89 12.20 -5 -3 0 118.69 10.30 -5 -3 0 121.39 11.20 5 -3 0 127.19 10.80 5 -3 0 110.79 10.50 -5 3 0 111.89 10.50 5 3 0 114.29 10.10 -5 3 0 125.99 11.30 -5 3 0 135.79 11.80 5 3 0 119.59 10.60 -5 3 0 119.09 11.00 5 3 0 131.09 10.40 5 3 0 115.29 10.60 -6 -3 0 80.19 8.80 -6 -3 0 55.09 6.80 6 -3 0 66.19 6.80 -6 -3 0 58.89 7.20 6 -3 0 41.30 6.40 6 -3 0 59.49 6.30 -6 -3 0 62.69 6.30 -6 3 0 49.10 6.20 -6 3 0 65.59 7.30 6 3 0 58.89 6.40 6 3 0 50.39 6.20 -6 3 0 53.79 6.80 -6 3 0 65.69 7.70 6 3 0 59.89 6.60 -7 -3 0 8.10 4.40 -7 -3 0 3.80 5.00 -7 -3 0 16.20 6.00 -7 -3 0 9.30 3.20 7 -3 0 -0.90 3.70 7 3 0 3.10 2.50 -7 3 0 3.20 4.30 -7 3 0 0.60 6.50 -7 3 0 -3.50 3.60 7 3 0 1.60 3.10 7 3 0 0.80 3.90 -7 3 0 8.80 5.10 -8 -3 0 -5.70 5.30 -8 -3 0 -0.90 4.90 -8 -3 0 3.10 3.10 8 -3 0 5.40 4.00 -8 3 0 -0.10 5.20 -8 3 0 -6.30 3.90 8 3 0 -5.40 4.40 8 3 0 4.10 3.20 -8 3 0 4.40 5.60 -9 -3 0 52.49 8.60 9 -3 0 42.00 7.30 9 -3 0 39.70 6.40 -9 -3 0 51.09 7.80 -9 3 0 38.60 7.40 -9 3 0 35.70 8.20 1 4 0 214.98 16.10 1 4 0 208.08 16.20 -2 4 0 9999.00 736.23 2 4 0 9567.64 736.33 3 -4 0 137.79 12.70 -3 -4 0 146.99 12.90 3 -4 0 165.18 12.70 -3 -4 0 155.98 12.90 -3 -4 0 163.38 12.90 3 -4 0 187.98 13.00 3 4 0 163.38 12.90 3 4 0 152.68 12.90 -3 4 0 154.28 12.80 3 4 0 163.98 12.90 -3 4 0 160.28 12.90 -3 4 0 160.58 12.90 3 4 0 167.48 12.40 -4 -4 0 292.47 23.60 4 -4 0 267.07 21.90 4 -4 0 284.47 22.00 -4 -4 0 283.77 22.10 4 4 0 298.37 22.00 -4 4 0 253.57 21.90 -4 4 0 267.67 22.50 4 4 0 292.87 22.00 -4 4 0 243.28 22.00 4 4 0 307.37 21.50 4 4 0 284.67 21.90 5 -4 0 56.29 7.30 -5 -4 0 104.19 9.60 -5 -4 0 73.49 8.00 5 -4 0 77.79 7.50 5 -4 0 78.99 7.90 -5 -4 0 85.59 8.50 -5 -4 0 76.19 7.40 -5 4 0 69.89 8.00 -5 4 0 83.99 8.50 -5 4 0 67.39 7.50 5 4 0 76.09 6.90 5 4 0 69.49 7.80 5 4 0 74.09 7.50 -5 4 0 95.59 8.90 5 4 0 74.19 7.60 6 -4 0 42.80 6.30 -6 -4 0 59.89 7.20 6 -4 0 72.09 7.60 -6 -4 0 41.00 6.40 6 -4 0 63.29 6.30 -6 -4 0 52.99 6.40 -6 -4 0 62.49 8.30 -6 4 0 63.89 7.60 6 4 0 56.09 6.30 -6 4 0 71.79 7.40 6 4 0 51.29 6.00 -6 4 0 60.59 6.40 -6 4 0 53.99 6.70 6 4 0 48.30 6.40 7 -4 0 6.20 4.00 -7 -4 0 -0.70 4.30 -7 -4 0 5.20 3.20 -7 -4 0 7.90 6.10 -7 -4 0 2.50 4.90 -7 4 0 6.30 5.20 7 4 0 5.50 4.20 -7 4 0 7.40 4.00 7 4 0 -1.30 2.70 -7 4 0 4.60 4.30 -8 -4 0 4.50 3.30 8 -4 0 0.10 4.10 -8 -4 0 1.60 5.00 -8 -4 0 4.60 5.80 8 4 0 -0.20 4.10 8 4 0 -3.60 2.90 -8 4 0 4.50 4.20 -8 4 0 -1.40 5.20 -8 4 0 -3.30 5.50 9 -4 0 -7.10 4.90 -9 -4 0 2.80 5.70 9 -4 0 7.00 4.50 -9 -4 0 1.90 3.40 -9 -4 0 1.40 6.20 -9 4 0 0.70 6.30 -9 4 0 4.90 6.00 0 -5 0 0.10 0.70 0 -5 0 0.60 0.70 0 -5 0 -0.20 0.70 0 -5 0 0.90 0.70 0 -5 0 1.10 0.80 0 5 0 -0.40 0.80 0 5 0 0.70 0.70 0 5 0 -0.70 0.80 -1 -5 0 345.67 26.30 -1 -5 0 337.57 26.40 1 -5 0 354.76 26.20 1 -5 0 341.07 26.20 -1 -5 0 327.07 26.10 1 -5 0 358.46 26.20 -1 -5 0 310.27 26.20 -1 5 0 371.86 26.30 -1 5 0 373.86 26.20 1 5 0 319.27 26.40 1 5 0 337.77 26.20 -1 5 0 335.07 26.20 1 5 0 352.36 26.30 1 5 0 351.66 26.10 2 -5 0 19.30 2.60 2 -5 0 13.40 2.30 2 -5 0 19.20 2.50 2 -5 0 13.60 2.20 2 5 0 14.00 2.20 -2 5 0 11.20 2.20 2 5 0 15.30 2.70 -2 5 0 12.70 2.30 -2 5 0 13.40 2.30 2 5 0 12.70 2.40 -3 -5 0 918.01 63.29 3 -5 0 853.51 63.19 3 -5 0 834.42 63.09 -3 -5 0 831.22 63.19 3 -5 0 760.72 62.99 -3 -5 0 796.52 63.09 3 5 0 836.62 63.09 -3 5 0 746.63 63.19 -3 5 0 843.32 63.19 3 5 0 810.12 63.29 3 5 0 855.01 62.69 -3 5 0 772.62 63.09 3 5 0 869.31 63.09 -3 5 0 914.81 63.39 -4 -5 0 629.24 45.70 4 -5 0 576.54 45.50 4 -5 0 558.64 45.30 -4 -5 0 610.44 45.60 -4 -5 0 666.53 45.50 4 -5 0 521.65 45.30 -4 5 0 607.94 45.90 -4 5 0 543.85 45.40 -4 5 0 530.65 45.40 4 5 0 629.04 45.50 4 5 0 623.94 45.00 4 5 0 633.94 45.40 -4 5 0 584.24 45.50 4 5 0 592.34 45.50 5 -5 0 1.10 2.80 -5 -5 0 3.40 3.30 5 -5 0 -0.50 2.80 -5 -5 0 3.10 4.50 -5 -5 0 3.60 3.40 -5 -5 0 4.90 3.00 5 -5 0 6.40 3.20 5 5 0 3.80 2.10 5 5 0 2.90 3.10 -5 5 0 1.00 3.60 -5 5 0 -0.60 3.60 -5 5 0 -0.50 3.10 -5 5 0 4.60 3.00 5 5 0 2.60 2.80 5 5 0 5.10 3.10 -6 -5 0 47.20 6.50 6 -5 0 32.30 5.40 6 -5 0 54.59 5.60 6 -5 0 53.39 6.20 -6 -5 0 50.39 7.70 -6 -5 0 49.20 5.50 -6 -5 0 41.00 5.90 -6 5 0 50.29 6.50 -6 5 0 56.89 6.70 -6 5 0 46.40 5.90 6 5 0 38.80 5.40 -6 5 0 46.50 6.80 6 5 0 36.00 4.60 6 5 0 31.50 5.60 -7 -5 0 18.60 6.40 -7 -5 0 10.90 4.70 -7 -5 0 6.00 5.20 -7 -5 0 7.70 3.50 7 -5 0 13.40 4.40 7 5 0 6.40 4.30 -7 5 0 14.00 4.70 -7 5 0 15.50 5.50 -7 5 0 9.10 4.30 -8 -5 0 16.50 5.60 8 -5 0 17.40 4.70 -8 -5 0 6.50 5.70 -8 -5 0 16.60 4.00 8 5 0 7.50 4.80 -8 5 0 9.20 5.70 -8 5 0 8.50 4.80 -8 5 0 16.60 6.40 9 -5 0 3.30 5.10 -9 -5 0 1.20 6.10 -9 -5 0 2.00 3.20 -9 -5 0 0.20 5.80 9 -5 0 -2.00 4.50 -9 5 0 -0.30 5.60 -9 5 0 -2.30 4.80 -9 5 0 -5.20 6.30 0 6 0 2331.27 182.68 0 6 0 2500.15 182.68 0 6 0 2360.36 182.68 0 6 0 2505.95 182.78 1 -6 0 954.50 68.59 -1 -6 0 881.71 68.69 -1 -6 0 878.71 68.59 1 -6 0 922.51 68.69 1 -6 0 963.30 68.59 -1 -6 0 827.62 68.59 1 -6 0 915.51 68.49 -1 -6 0 870.61 68.39 1 6 0 930.81 68.59 1 6 0 890.31 68.59 -1 6 0 905.11 68.59 1 6 0 870.01 68.79 1 6 0 938.91 68.49 -1 6 0 974.50 68.59 -1 6 0 860.01 68.49 -1 6 0 927.01 68.49 2 -6 0 12.40 2.30 -2 -6 0 19.10 2.50 2 -6 0 12.70 2.30 2 -6 0 15.80 2.30 -2 -6 0 16.50 2.40 2 -6 0 16.00 2.30 -2 6 0 13.20 2.50 -2 6 0 7.40 2.20 2 6 0 20.40 2.40 2 6 0 23.30 2.70 -2 6 0 12.20 2.30 -2 6 0 12.50 2.20 2 6 0 17.00 1.70 3 -6 0 14.80 2.80 3 -6 0 15.20 3.10 -3 -6 0 15.40 3.10 3 -6 0 18.10 3.30 -3 -6 0 19.60 3.00 3 -6 0 12.90 2.70 -3 -6 0 18.90 3.40 -3 6 0 17.40 2.80 3 6 0 18.80 3.00 -3 6 0 18.20 2.90 3 6 0 23.20 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145.79 13.50 4 -20 0 137.19 12.00 4 -20 0 109.59 10.90 4 -20 0 136.59 12.00 4 -20 0 118.09 12.50 -4 -20 0 129.09 12.50 4 -20 0 120.49 11.90 -4 -20 0 128.79 13.30 4 20 0 137.89 12.60 -4 20 0 121.89 13.40 4 20 0 132.19 11.10 4 20 0 125.09 13.50 -4 20 0 124.19 12.50 -4 20 0 123.39 11.80 -4 20 0 131.49 12.70 4 20 0 131.99 12.30 5 -20 0 -3.20 4.20 -5 -20 0 11.90 5.50 5 -20 0 13.20 2.70 5 -20 0 11.60 4.70 5 -20 0 5.40 4.20 -5 -20 0 14.30 5.30 5 -20 0 8.40 5.30 -5 -20 0 5.70 5.20 5 20 0 14.30 6.00 -5 20 0 9.40 5.50 5 20 0 1.10 5.20 -5 20 0 6.20 5.30 -5 20 0 1.70 5.40 -5 20 0 4.70 4.40 5 20 0 5.90 4.80 -6 -20 0 98.79 11.70 6 -20 0 107.09 11.20 -6 -20 0 109.49 12.40 6 -20 0 123.79 12.30 -6 -20 0 102.99 12.40 -6 20 0 129.09 12.70 -6 20 0 105.39 11.80 -6 20 0 89.99 11.70 -6 20 0 103.39 12.30 6 20 0 110.79 11.90 7 -20 0 66.99 8.10 -7 -20 0 67.29 9.40 -7 -20 0 55.69 8.70 -7 -20 0 61.79 9.60 7 20 0 39.30 8.40 -7 20 0 64.99 9.20 -7 20 0 70.39 8.90 -7 20 0 44.10 8.20 8 -20 0 23.60 6.40 -8 -20 0 42.00 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33.10 2 22 0 473.75 32.50 -2 22 0 406.26 32.10 -2 22 0 413.66 32.90 -2 22 0 391.06 33.10 2 22 0 440.06 33.00 3 -22 0 17.10 4.80 3 -22 0 18.40 4.30 -3 -22 0 22.70 5.40 -3 -22 0 18.90 5.50 3 -22 0 18.70 4.30 3 -22 0 18.70 4.60 -3 -22 0 20.20 5.70 3 -22 0 20.80 4.70 3 22 0 26.10 6.10 3 22 0 13.10 5.50 -3 22 0 13.30 4.90 -3 22 0 17.40 4.10 3 22 0 15.50 4.90 3 22 0 17.20 4.20 -3 22 0 14.60 5.40 -3 22 0 25.00 6.00 4 -22 0 66.49 9.60 4 -22 0 77.39 7.80 4 -22 0 79.59 8.40 -4 -22 0 50.49 8.60 -4 -22 0 80.09 9.50 4 -22 0 69.39 8.40 4 -22 0 71.89 8.30 -4 -22 0 90.09 9.70 4 22 0 68.69 9.10 4 22 0 89.99 10.50 -4 22 0 73.49 9.80 4 22 0 76.69 7.90 -4 22 0 69.59 8.70 4 22 0 78.79 8.80 -4 22 0 79.39 9.00 -4 22 0 79.49 9.30 5 -22 0 39.50 4.90 -5 -22 0 38.30 6.80 5 -22 0 32.80 6.50 -5 -22 0 58.99 8.10 5 -22 0 46.90 6.60 5 -22 0 46.80 6.60 -5 -22 0 44.10 7.90 5 -22 0 46.00 6.60 -5 22 0 36.00 6.20 5 22 0 44.30 7.10 -5 22 0 31.10 7.30 5 22 0 38.90 6.90 5 22 0 51.59 8.30 -5 22 0 36.10 6.80 -5 22 0 44.30 7.70 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12.10 -2 -23 0 116.59 12.30 2 -23 0 118.49 11.70 2 -23 0 112.39 10.90 2 -23 0 90.59 11.00 -2 -23 0 131.39 12.10 2 -23 0 121.49 11.50 -2 -23 0 119.49 12.00 -2 23 0 101.49 12.30 2 23 0 137.19 12.20 -2 23 0 118.09 12.10 2 23 0 106.59 11.70 -2 23 0 105.89 10.50 2 23 0 117.49 12.50 -2 23 0 117.99 11.50 -3 -23 0 11.80 5.00 3 -23 0 24.00 5.60 3 -23 0 24.60 5.00 -3 -23 0 29.50 6.30 -3 -23 0 12.20 4.80 -3 -23 0 22.50 3.90 3 -23 0 18.20 4.30 3 -23 0 13.50 4.80 3 -23 0 18.20 4.50 -3 23 0 20.20 5.20 3 23 0 12.50 4.90 -3 23 0 22.90 4.30 3 23 0 18.80 6.20 3 23 0 15.00 5.80 -3 23 0 7.90 5.00 3 23 0 19.20 4.40 -3 23 0 8.90 5.80 4 -23 0 4.60 4.80 -4 -23 0 4.00 5.20 4 -23 0 5.10 4.70 -4 -23 0 8.20 5.80 4 -23 0 12.00 4.40 4 -23 0 3.50 5.20 4 -23 0 10.70 3.80 -4 23 0 3.20 5.70 4 23 0 6.30 6.00 4 23 0 3.50 3.40 4 23 0 4.40 5.00 -4 23 0 10.80 5.00 4 23 0 6.80 5.50 -4 23 0 0.70 5.20 5 -23 0 24.20 5.80 -5 -23 0 20.30 6.00 5 -23 0 31.60 5.80 -5 -23 0 22.70 6.80 5 -23 0 14.50 5.40 5 -23 0 21.20 3.90 5 -23 0 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9.30 0 28 5 58.29 8.70 0 28 -5 62.79 9.30 1 -28 5 37.30 7.30 1 -28 5 71.29 10.70 1 -28 5 55.69 8.70 -1 -28 -5 37.30 7.20 -1 -28 -5 49.30 7.70 1 -28 5 56.49 8.40 1 -28 5 62.09 8.40 -1 -28 -5 59.99 10.20 -1 28 -5 42.90 7.50 1 28 5 59.29 8.40 -1 28 -5 38.10 7.10 -1 28 -5 75.09 9.50 1 28 5 54.09 8.90 1 28 5 48.80 8.20 -1 28 -5 56.69 8.70 1 28 5 49.99 8.90 2 -28 5 12.90 6.80 2 -28 5 11.80 5.70 -2 -28 -5 11.50 5.30 2 -28 5 13.00 7.10 -2 -28 -5 10.10 6.60 -2 -28 -5 5.00 5.40 2 28 5 -0.30 5.80 -2 28 -5 23.70 7.40 -2 28 -5 0.40 5.10 2 28 5 5.70 7.20 2 28 5 10.00 7.30 -2 28 -5 6.70 5.70 2 28 5 18.80 6.30 3 -28 5 -4.70 6.70 3 -28 5 4.70 5.00 -3 -28 -5 12.40 7.00 3 -28 5 18.10 6.00 -3 -28 -5 5.90 6.40 3 -28 5 -7.20 6.40 -3 28 -5 1.50 6.40 -3 28 -5 0.00 5.90 3 28 5 1.10 7.00 -3 28 -5 0.90 6.00 3 28 5 -1.20 7.40 3 28 5 8.60 6.20 -3 28 -5 8.60 7.30 3 28 5 -1.50 5.70 4 -28 5 2.80 5.10 4 -28 5 -5.30 6.90 -4 -28 -5 2.10 7.20 -4 -28 -5 8.40 6.90 4 -28 5 0.90 7.20 4 28 5 -3.50 6.70 -4 28 -5 4.10 6.50 4 28 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29 5 6.70 5.80 -4 29 5 8.20 6.10 4 29 -5 16.30 4.70 4 29 -5 12.20 6.40 3 -29 -5 2.80 4.70 -3 -29 5 9.80 7.50 -3 -29 5 3.00 6.80 -3 -29 5 7.90 5.90 3 -29 -5 7.00 4.80 -3 -29 5 4.70 3.80 -3 29 5 3.10 10.10 3 29 -5 11.70 6.40 3 29 -5 3.20 4.60 -3 29 5 -4.30 5.60 -3 29 5 10.10 7.40 -3 29 5 10.20 6.20 -2 -29 5 1.10 4.20 2 -29 -5 2.20 4.60 -2 -29 5 1.50 6.40 -2 -29 5 -1.20 6.20 2 -29 -5 8.10 5.20 -2 29 5 -5.30 5.30 -2 29 5 1.60 5.60 2 29 -5 -7.70 5.50 -2 29 5 -1.30 6.20 2 29 -5 6.00 5.00 2 29 -5 -3.50 5.40 -2 29 5 0.20 6.20 -1 -29 5 5.00 5.80 1 -29 -5 6.50 5.30 -1 -29 5 2.40 5.90 1 -29 -5 1.80 4.80 -1 -29 5 -0.10 6.30 -1 -29 5 4.10 6.60 1 29 -5 -5.50 5.30 -1 29 5 16.80 7.00 -1 29 5 -2.20 5.40 -1 29 5 -4.40 6.10 -1 29 5 4.20 6.20 1 29 -5 -2.00 5.40 0 -29 5 174.08 16.00 0 -29 -5 140.89 14.70 0 -29 5 147.09 16.70 0 -29 -5 164.58 15.20 0 -29 -5 159.38 13.50 0 -29 5 161.68 15.80 0 -29 5 171.78 16.10 0 -29 -5 128.39 15.60 0 29 5 143.49 16.30 0 29 5 164.98 16.40 0 29 -5 143.19 15.60 0 29 -5 163.78 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4 9 138.99 14.50 -5 4 9 150.98 14.50 -4 -4 9 240.98 22.40 -4 -4 9 293.77 22.20 -4 -4 9 264.67 20.10 -4 -4 9 259.07 20.20 -4 4 9 245.08 21.70 -4 4 9 262.07 19.80 -4 4 9 240.88 19.70 -4 4 9 254.97 21.40 -4 4 9 250.57 21.60 -3 -4 9 1904.71 146.09 3 -4 -9 1975.10 144.79 3 -4 -9 1962.10 144.89 3 -4 -9 1784.72 145.79 -3 -4 9 1933.41 146.39 -3 -4 9 1861.01 145.09 -3 -4 9 1874.41 145.19 -3 4 9 2015.40 146.09 3 4 -9 1919.81 146.29 -3 4 9 1899.71 145.79 -3 4 9 1842.92 145.09 3 4 -9 1963.40 144.99 3 4 -9 1948.31 144.99 -3 4 9 1998.40 145.09 -2 -4 9 94.69 9.50 -2 -4 9 93.69 11.00 2 -4 -9 110.29 10.30 -2 -4 9 81.89 10.90 2 -4 -9 102.89 8.90 2 -4 -9 105.09 8.90 -2 -4 9 99.29 9.60 -2 4 9 104.59 10.50 2 4 -9 89.89 9.00 -2 4 9 110.49 9.50 -2 4 9 99.29 10.90 -2 4 9 103.19 9.40 2 4 -9 96.79 9.20 2 4 -9 97.79 10.70 -1 -4 9 609.34 54.59 1 -4 -9 700.03 53.69 1 -4 -9 771.02 54.39 -1 -4 9 711.13 54.09 -1 -4 9 688.93 54.39 1 -4 -9 754.52 54.39 -1 -4 9 681.63 54.59 1 -4 -9 739.33 53.69 -1 4 9 779.02 54.09 -1 4 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67.99 8.40 2 5 -9 57.69 6.40 -2 5 9 73.39 7.50 2 5 -9 61.89 7.90 -2 5 9 63.49 7.20 -1 -5 9 13.60 4.70 1 -5 -9 18.60 4.30 1 -5 -9 15.90 3.80 -1 -5 9 21.20 5.70 1 -5 -9 27.70 5.00 -1 -5 9 11.80 4.10 -1 -5 9 18.80 4.90 -1 -5 9 18.10 5.20 1 -5 -9 26.10 3.90 -1 5 9 30.50 5.70 -1 5 9 19.00 4.60 -1 5 9 20.80 5.80 1 5 -9 12.60 4.80 -1 5 9 20.20 4.40 1 5 -9 6.40 3.60 0 -5 -9 3.80 3.70 0 -5 -9 2.70 4.30 0 -5 9 8.20 3.90 0 -5 -9 -2.10 3.40 0 -5 9 5.20 4.80 0 -5 9 -2.20 3.90 0 -5 -9 11.40 4.40 0 -5 9 -2.50 4.30 0 -5 9 0.80 4.30 0 5 9 2.70 5.00 0 5 9 -6.80 3.90 0 5 -9 10.00 4.10 0 5 9 5.70 4.60 0 5 -9 3.70 3.60 0 5 -9 -2.80 4.20 0 5 9 1.10 3.80 1 -5 9 24.70 6.10 -1 -5 -9 29.80 5.10 1 -5 9 26.70 6.00 -1 -5 -9 22.20 4.60 -1 -5 -9 39.80 7.10 1 -5 9 17.60 5.70 1 -5 9 16.20 6.10 -1 -5 -9 32.10 5.20 1 -5 9 15.80 5.30 -1 5 -9 30.40 6.40 1 5 9 32.70 5.70 -1 5 -9 24.60 5.50 -1 5 -9 22.10 5.20 1 5 9 34.30 6.20 1 5 9 34.10 6.30 1 5 9 30.00 6.50 -2 -5 -9 -1.60 4.60 -2 -5 -9 8.30 8.80 -2 -5 -9 -3.40 5.80 -2 -5 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14.60 8.40 6 5 9 1.30 8.20 -6 5 -9 11.80 8.80 6 5 9 12.90 6.70 -9 -6 9 171.68 16.40 -9 -6 9 115.69 14.10 -9 -6 9 139.19 17.40 -9 6 9 130.89 15.90 -9 6 9 137.99 15.20 -9 6 9 146.99 13.30 -8 -6 9 46.70 5.40 -8 -6 9 53.49 6.60 -8 -6 9 47.40 7.80 -8 -6 9 55.69 10.80 -8 6 9 58.49 9.30 -8 6 9 48.60 7.40 -8 6 9 66.69 9.40 -7 -6 9 33.20 6.70 -7 -6 9 35.50 9.50 -7 6 9 48.50 8.10 -7 6 9 33.70 6.60 -7 6 9 38.50 7.80 -6 -6 9 29.40 6.40 -6 -6 9 22.90 7.60 -6 -6 9 20.60 4.80 -6 6 9 18.90 5.50 -6 6 9 8.40 5.20 -6 6 9 12.80 5.60 -5 -6 9 14.60 6.90 -5 -6 9 16.70 6.00 -5 -6 9 18.10 2.90 -5 6 9 17.70 5.50 -5 6 9 11.80 4.80 -5 6 9 17.30 5.40 -4 -6 9 30.80 4.00 -4 -6 9 36.70 7.10 -4 -6 9 32.30 4.40 -4 -6 9 37.80 6.70 -4 6 9 26.70 5.60 -4 6 9 20.90 5.60 -4 6 9 25.30 3.30 -4 6 9 22.40 5.90 4 6 -9 29.10 3.20 -4 6 9 28.60 3.40 4 6 -9 25.10 3.40 -3 -6 9 358.86 29.00 -3 -6 9 386.56 30.30 3 -6 -9 349.77 28.50 3 -6 -9 342.57 28.40 -3 -6 9 418.96 31.10 -3 -6 9 414.06 29.20 -3 6 9 376.76 30.10 3 6 -9 396.86 28.80 3 6 -9 392.76 28.70 3 6 -9 417.96 30.60 -3 6 9 333.47 28.70 -3 6 9 314.27 29.50 -2 -6 9 64.49 7.10 2 -6 -9 56.79 6.80 2 -6 -9 52.29 5.80 -2 -6 9 74.49 8.90 -2 -6 9 68.09 6.80 -2 -6 9 81.89 8.40 2 -6 -9 49.10 5.70 2 -6 -9 51.49 7.00 -2 -6 9 51.19 7.10 2 6 -9 69.39 6.70 -2 6 9 49.99 7.50 -2 6 9 51.09 10.40 -2 6 9 54.89 6.40 2 6 -9 60.19 6.40 2 6 -9 78.19 8.70 -2 6 9 52.39 6.30 -1 -6 9 148.99 14.30 1 -6 -9 127.29 12.20 -1 -6 9 166.88 14.10 -1 -6 9 130.59 12.80 -1 -6 9 174.08 13.20 1 -6 -9 132.49 12.30 1 -6 -9 138.09 13.20 1 -6 -9 137.29 13.10 -1 6 9 122.79 12.50 -1 6 9 131.39 14.00 1 6 -9 155.48 13.70 1 6 -9 160.08 12.40 -1 6 9 152.48 12.90 -1 6 9 132.49 13.50 0 -6 9 92.39 10.50 0 -6 9 81.59 8.90 0 -6 -9 63.79 8.00 0 -6 9 94.79 9.60 0 -6 9 103.89 8.90 0 -6 -9 76.79 8.60 0 -6 9 96.99 9.20 0 -6 -9 58.59 7.70 0 -6 -9 70.49 8.20 0 6 9 72.39 9.30 0 6 9 53.59 7.90 0 6 -9 89.79 9.00 0 6 -9 97.79 8.70 0 6 9 56.69 8.80 0 6 9 64.19 8.30 0 6 -9 86.99 9.60 1 -6 9 3.50 5.30 -1 -6 -9 8.60 5.50 1 -6 9 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115.49 10.40 0 -7 10 101.19 11.20 0 -7 -10 83.39 9.00 0 -7 10 103.49 10.90 0 -7 -10 77.69 9.20 0 7 -10 91.19 11.10 0 7 10 83.49 9.70 0 7 -10 92.49 10.00 0 7 10 103.29 11.00 0 7 -10 93.99 9.40 0 7 10 81.29 9.50 0 7 10 78.69 10.30 -1 -7 -10 121.49 13.60 1 -7 10 128.19 15.80 -1 -7 -10 138.29 13.10 -1 -7 -10 120.89 12.80 1 -7 10 146.99 14.10 1 -7 10 123.59 13.50 -1 -7 -10 131.29 15.30 1 -7 10 162.28 14.70 -1 7 -10 140.69 13.50 1 7 10 128.09 13.20 1 7 10 143.39 14.90 1 7 10 158.88 14.10 1 7 10 148.29 14.90 -1 7 -10 139.99 14.60 -1 7 -10 126.99 13.00 2 -7 10 75.99 10.00 -2 -7 -10 76.49 9.30 -2 -7 -10 97.69 11.30 -2 -7 -10 74.99 9.20 -2 -7 -10 81.39 12.90 2 -7 10 70.59 9.50 2 -7 10 78.19 9.90 2 7 10 73.29 9.80 2 7 10 60.99 10.50 2 7 10 72.79 9.50 -2 7 -10 74.79 9.10 2 7 10 83.19 10.10 -2 7 -10 76.19 9.80 3 -7 10 28.60 8.80 3 -7 10 35.10 8.60 3 -7 10 44.50 7.90 3 -7 10 34.50 7.30 -3 -7 -10 46.40 8.10 3 7 10 74.09 12.90 3 7 10 36.60 7.10 3 7 10 53.79 14.40 3 7 10 46.40 8.40 -4 -7 -10 10.20 6.90 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6.60 5.30 4 8 -10 10.40 3.10 4 8 -10 5.30 2.60 -4 8 10 0.00 5.00 -3 -8 10 4.00 5.30 -3 -8 10 8.50 3.90 -3 -8 10 7.00 4.20 -3 -8 10 17.00 5.70 3 -8 -10 6.30 3.80 3 -8 -10 4.00 2.50 -3 -8 10 1.70 3.60 3 -8 -10 7.50 2.90 -3 8 10 4.00 3.50 3 8 -10 12.10 6.30 -3 8 10 7.80 3.50 3 8 -10 7.80 3.20 3 8 -10 6.40 3.00 -3 8 10 8.50 4.40 -3 8 10 10.20 5.40 -2 -8 10 15.90 4.60 -2 -8 10 2.60 5.80 -2 -8 10 9.90 4.60 -2 -8 10 10.20 6.00 2 -8 -10 8.10 8.10 2 -8 -10 9.00 3.30 -2 -8 10 6.30 3.90 2 -8 -10 10.20 3.30 2 -8 -10 8.10 4.30 -2 8 10 9.20 4.20 -2 8 10 3.40 4.60 -2 8 10 4.90 5.10 -2 8 10 -3.60 3.70 2 8 -10 8.10 3.70 2 8 -10 10.20 3.40 2 8 -10 14.90 4.80 1 -8 -10 29.10 4.80 1 -8 -10 19.30 5.10 -1 -8 10 34.90 6.80 1 -8 -10 26.00 5.50 1 -8 -10 24.90 5.60 -1 -8 10 48.90 6.40 -1 -8 10 48.00 6.00 -1 -8 10 53.29 7.00 -1 8 10 23.90 5.60 -1 8 10 36.50 6.80 -1 8 10 26.50 6.10 -1 8 10 28.10 7.90 0 -8 10 211.18 21.50 0 -8 -10 219.38 19.70 0 -8 -10 214.88 19.70 0 -8 10 260.07 20.70 0 -8 10 270.17 20.60 0 -8 10 261.37 21.30 0 -8 10 260.97 20.90 0 -8 -10 220.98 20.20 0 -8 -10 234.08 20.60 0 8 -10 260.77 20.00 0 8 10 225.08 20.40 0 8 10 242.18 21.50 0 8 -10 283.67 20.10 0 8 -10 240.08 21.10 0 8 10 200.38 20.70 0 8 10 223.78 20.50 1 -8 10 124.99 12.50 -1 -8 -10 84.99 9.90 1 -8 10 81.39 10.00 -1 -8 -10 90.29 10.80 1 -8 10 107.49 12.50 1 -8 10 115.29 12.10 -1 -8 -10 108.89 11.90 -1 -8 -10 96.29 10.70 1 8 10 87.29 10.50 1 8 10 110.09 12.60 1 8 10 97.79 11.50 -1 8 -10 97.59 10.60 -1 8 -10 105.19 12.20 -1 8 -10 108.09 11.10 1 8 10 69.69 9.80 2 -8 10 10.40 6.10 2 -8 10 20.10 8.10 2 -8 10 9.70 5.70 -2 -8 -10 28.70 7.90 -2 -8 -10 14.30 5.80 2 -8 10 11.60 6.30 -2 -8 -10 7.30 5.30 2 8 10 19.10 6.70 2 8 10 18.80 7.00 2 8 10 9.80 6.40 2 8 10 13.00 6.70 -2 8 -10 13.30 6.30 -2 8 -10 18.70 5.50 3 -8 10 22.00 6.70 3 -8 10 11.20 7.30 -3 -8 -10 10.30 6.50 3 -8 10 5.70 5.60 3 -8 10 16.30 7.70 3 8 10 30.00 7.70 3 8 10 14.00 6.00 3 8 10 26.40 12.80 3 8 10 22.60 12.40 -3 8 -10 8.80 6.90 4 -8 10 -5.50 7.40 -4 -8 -10 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-14 8.70 5.00 -2 10 14 9.40 6.90 -2 10 14 5.50 5.60 -2 10 14 8.20 7.90 -1 -10 14 3.60 8.10 -1 -10 14 7.90 8.30 1 -10 -14 -0.90 4.30 -1 -10 14 -9.50 6.70 -1 -10 14 5.80 6.50 -1 10 14 16.90 7.10 -1 10 14 5.60 6.20 -1 10 14 1.00 7.50 1 10 -14 -2.50 4.90 -1 10 14 2.60 6.70 0 -10 14 9.70 7.80 0 -10 -14 10.50 5.60 0 -10 14 16.00 7.40 0 -10 14 -0.70 8.70 0 -10 14 5.80 7.40 0 10 14 -2.30 6.90 0 10 -14 4.40 6.00 0 10 14 7.80 6.80 0 10 14 1.60 7.80 0 10 14 10.60 7.60 -5 -11 14 -9.10 9.00 -5 -11 14 -2.40 4.50 -5 -11 14 2.10 8.40 -5 11 14 12.30 8.20 -5 11 14 -3.20 2.90 -5 11 14 -3.80 7.40 -5 11 14 1.30 5.80 -4 -11 14 46.20 7.50 -4 -11 14 41.90 11.20 -4 -11 14 46.90 7.50 4 -11 -14 51.29 5.60 -4 -11 14 52.49 11.10 -4 11 14 45.80 7.00 -4 11 14 56.59 10.90 -4 11 14 73.29 8.90 -4 11 14 61.39 6.80 -4 11 14 35.40 9.50 4 11 -14 47.00 6.10 -3 -11 14 22.90 6.60 -3 -11 14 26.60 6.90 -3 -11 14 28.40 9.60 3 -11 -14 19.40 6.80 -3 -11 14 22.00 9.40 3 -11 -14 39.00 5.70 -3 11 14 41.60 6.50 3 11 -14 17.10 5.20 -3 11 14 34.40 9.70 -3 11 14 23.90 8.40 -3 11 14 31.90 6.40 -3 11 14 37.10 7.50 2 -11 -14 107.09 14.30 -2 -11 14 152.28 15.20 2 -11 -14 133.19 12.90 -2 -11 14 144.69 14.30 -2 -11 14 150.98 16.40 -2 -11 14 148.09 17.30 -2 11 14 127.19 14.00 -2 11 14 144.59 15.20 2 11 -14 122.99 13.30 -2 11 14 129.49 15.50 -1 -11 14 5.60 8.20 -1 -11 14 -3.90 6.20 -1 -11 14 -4.10 6.90 1 -11 -14 10.50 4.90 -1 -11 14 0.30 7.60 -1 11 14 12.00 6.60 1 11 -14 11.20 5.30 -1 11 14 1.10 7.90 -1 11 14 7.70 7.10 0 -11 14 99.69 12.50 0 -11 14 124.29 16.20 0 -11 14 87.39 12.80 0 -11 -14 79.09 10.30 0 -11 14 90.59 12.10 0 11 14 91.19 13.70 0 11 14 113.09 12.40 0 11 -14 76.79 11.00 0 11 14 130.69 14.60 0 11 14 90.19 11.60 -4 -12 14 23.70 6.10 -4 -12 14 22.40 9.40 -4 -12 14 12.40 10.10 -4 -12 14 32.10 6.60 -4 12 14 20.30 5.50 4 12 -14 18.30 4.50 -4 12 14 30.10 9.10 -4 12 14 18.10 5.30 -4 12 14 20.90 9.10 -4 12 14 13.70 6.10 -3 -12 14 8.10 8.90 -3 -12 14 9.30 6.20 3 -12 -14 3.60 5.60 -3 -12 14 -3.20 8.40 -3 -12 14 4.90 5.90 3 -12 -14 -0.50 4.40 -3 12 14 5.40 8.30 -3 12 14 1.60 5.10 3 12 -14 0.10 4.40 -3 12 14 8.30 6.40 -3 12 14 8.50 5.30 -3 12 14 7.00 7.50 -2 -12 14 14.60 5.90 -2 -12 14 1.80 8.00 2 -12 -14 -4.50 4.40 -2 -12 14 4.70 8.30 2 -12 -14 3.90 5.70 -2 -12 14 2.80 6.30 2 12 -14 4.40 5.20 -2 12 14 10.70 6.40 -2 12 14 4.70 5.50 -2 12 14 2.40 5.80 -2 12 14 -0.40 7.60 -1 -12 14 4.40 8.20 -1 -12 14 11.00 9.30 1 -12 -14 -3.00 5.80 -1 -12 14 5.60 7.40 -1 -12 14 18.90 6.90 1 -12 -14 9.10 4.90 -1 12 14 12.50 6.80 1 12 -14 16.90 6.00 -1 12 14 12.20 8.20 -1 12 14 9.90 6.50 -1 12 14 3.60 6.20 0 -12 14 -6.40 7.70 0 -12 14 7.80 7.00 0 -12 14 2.70 7.80 0 -12 14 0.00 9.80 0 -12 -14 3.40 5.30 0 12 14 14.40 7.20 0 12 14 9.30 7.00 0 12 -14 4.80 6.50 0 12 14 19.90 9.50 0 12 14 28.40 7.80 -4 -13 14 2.10 5.30 -4 -13 14 7.00 5.70 -4 -13 14 7.80 8.00 4 -13 -14 9.80 3.30 -4 -13 14 1.00 9.20 -4 13 14 5.50 8.00 -4 13 14 16.20 5.80 4 13 -14 3.70 4.10 -4 13 14 2.80 7.50 -4 13 14 7.90 4.80 -4 13 14 4.50 5.20 3 -13 -14 61.19 9.00 -3 -13 14 66.59 9.00 3 -13 -14 63.09 8.30 -3 -13 14 61.19 12.10 -3 -13 14 92.69 12.80 -3 13 14 68.89 12.00 -3 13 14 62.49 11.10 3 13 -14 65.19 8.00 -3 13 14 66.29 8.90 -3 13 14 85.39 9.60 -3 13 14 73.79 8.80 -2 -13 14 -3.40 8.10 -2 -13 14 -10.10 7.30 2 -13 -14 -2.20 5.80 -2 -13 14 1.50 10.00 2 -13 -14 -1.40 4.50 -2 -13 14 -8.10 6.40 -2 13 14 -8.90 7.40 -2 13 14 0.90 7.60 -2 13 14 5.10 6.20 -2 13 14 4.10 6.00 -2 13 14 6.40 5.30 2 13 -14 4.70 5.10 1 -13 -14 7.40 6.00 -1 -13 14 -10.60 8.40 -1 -13 14 4.30 6.60 -1 -13 14 -9.70 6.90 -1 -13 14 2.50 8.00 1 -13 -14 4.70 4.80 1 13 -14 0.80 5.90 -1 13 14 -1.50 7.80 -1 13 14 10.00 6.50 -1 13 14 3.50 6.00 0 -13 14 5.10 7.40 0 13 14 9.90 7.50 -4 -14 14 -4.00 8.60 -4 -14 14 10.40 8.40 4 -14 -14 12.30 3.40 -4 -14 14 5.70 5.40 -4 -14 14 -0.40 5.60 4 14 -14 -2.90 4.60 -4 14 14 6.60 5.50 -4 14 14 -3.40 4.40 -4 14 14 -7.10 8.00 -4 14 14 3.00 5.10 -4 14 14 5.30 8.40 -3 -14 14 0.60 9.30 -3 -14 14 7.60 8.80 3 -14 -14 8.60 5.10 -3 -14 14 21.10 6.90 3 -14 -14 1.40 5.20 -3 -14 14 17.30 5.80 -3 14 14 4.90 7.40 -3 14 14 8.10 5.60 -3 14 14 13.50 6.00 -3 14 14 6.70 5.60 -3 14 14 10.70 8.90 3 14 -14 9.10 4.70 -2 -14 14 6.50 8.60 -2 -14 14 4.50 6.70 2 -14 -14 -7.30 4.40 -2 -14 14 8.20 9.90 -2 -14 14 7.50 9.00 -2 14 14 7.50 6.00 -2 14 14 8.90 6.40 -2 14 14 -1.30 8.10 -2 14 14 8.50 8.00 2 14 -14 5.20 5.20 -2 14 14 6.00 5.50 -1 -14 14 -8.00 8.30 -1 -14 14 -1.60 8.80 1 -14 -14 4.20 5.80 -1 -14 14 -1.40 7.30 -1 -14 14 6.90 6.90 1 -14 -14 -9.40 4.80 -1 14 14 2.60 6.40 -1 14 14 12.40 6.50 1 14 -14 -2.70 5.70 -1 14 14 3.50 5.90 -1 14 14 13.60 9.10 3 -15 -14 -0.80 5.10 -3 -15 14 0.00 9.50 3 -15 -14 -2.50 5.00 -3 -15 14 7.20 6.30 -3 -15 14 7.70 8.40 -3 -15 14 -2.50 6.20 -3 15 14 -2.40 5.40 -3 15 14 -6.00 7.10 -3 15 14 17.00 5.90 3 15 -14 -0.50 4.50 -3 15 14 4.70 5.50 -3 15 14 1.00 7.70 2 -15 -14 90.29 10.80 -2 -15 14 95.99 11.60 2 -15 -14 88.29 10.00 -2 -15 14 112.89 16.00 -2 -15 14 93.09 13.70 -2 -15 14 112.29 11.80 -2 15 14 87.79 12.80 -2 15 14 92.89 10.80 -2 15 14 95.69 13.70 -2 15 14 93.89 11.30 2 15 -14 84.99 10.30 1 -15 -14 15.00 6.40 -1 -15 14 18.00 8.20 -1 -15 14 8.30 9.20 -1 -15 14 17.00 9.50 -1 15 14 24.40 7.20 -1 15 14 30.00 7.40 -1 15 14 24.20 10.10 -1 15 14 17.30 8.80 1 15 -14 16.80 6.60 -3 -16 14 -5.00 8.60 3 -16 -14 6.40 5.20 -3 -16 14 2.20 6.30 -3 16 14 7.20 9.10 -3 16 14 9.60 8.50 -2 -16 14 6.40 7.10 2 -16 -14 10.20 6.10 -2 -16 14 1.20 8.90 -2 -16 14 -3.30 8.70 -2 16 14 16.00 6.20 -2 16 14 10.10 6.20 2 16 -14 9.30 5.50 -2 16 14 2.90 8.40 -2 16 14 3.00 8.80 -4 0 15 3.20 8.40 -4 0 15 0.40 4.40 -3 0 15 10.40 7.60 -3 0 15 15.10 5.40 -3 0 15 10.60 5.60 -3 0 15 15.00 8.90 3 0 -15 11.30 4.20 2 0 -15 -4.20 4.50 -2 0 15 8.20 5.80 -2 0 15 -8.40 8.60 -2 0 15 0.40 6.00 -2 0 15 0.20 7.20 -1 0 15 11.70 9.10 -1 0 15 -1.60 7.30 -4 -1 15 5.50 4.50 -4 -1 15 6.20 9.10 -4 1 15 8.90 4.60 -4 1 15 2.90 8.10 -3 -1 15 -5.60 6.80 3 -1 -15 0.80 4.00 -3 -1 15 1.50 5.20 -3 -1 15 8.90 5.10 -3 -1 15 -7.80 7.80 3 1 -15 1.70 3.90 -3 1 15 6.80 9.30 -3 1 15 2.90 5.20 -3 1 15 -4.40 7.30 -3 1 15 7.10 5.00 -2 -1 15 -3.70 6.10 -2 -1 15 -1.20 7.80 2 -1 -15 -2.90 4.30 -2 -1 15 6.80 7.50 -2 -1 15 5.90 5.30 -2 1 15 9.30 5.40 -2 1 15 -2.50 7.00 2 1 -15 -5.30 4.20 -2 1 15 3.80 6.20 -2 1 15 -1.50 8.60 -1 -1 15 63.39 9.80 -1 -1 15 52.99 10.90 -1 1 15 57.79 11.10 -1 1 15 49.00 9.30 -3 -2 15 2.40 5.40 -3 -2 15 -0.20 8.60 -3 -2 15 -2.70 6.50 3 -2 -15 -4.30 3.80 -3 2 15 -3.90 4.80 -3 2 15 6.30 9.10 3 2 -15 3.60 4.10 -3 2 15 3.80 7.00 -3 2 15 4.50 5.10 2 -2 -15 25.00 5.60 -2 -2 15 47.80 10.00 -2 -2 15 47.70 7.40 -2 -2 15 38.30 8.10 -2 -2 15 64.49 11.60 -2 2 15 33.40 6.80 -2 2 15 21.20 9.70 2 2 -15 26.10 5.80 -2 2 15 42.10 7.70 -2 2 15 34.20 8.80 -1 -2 15 0.60 6.90 -1 -2 15 21.10 9.60 -1 2 15 0.30 6.90 -1 2 15 10.30 9.00 3 -3 -15 -7.10 3.70 -3 -3 15 -1.00 5.30 -3 -3 15 8.70 5.50 -3 -3 15 -2.70 7.20 -3 -3 15 10.60 8.00 -3 3 15 -13.60 6.60 -3 3 15 0.50 8.70 -3 3 15 0.90 5.00 -3 3 15 4.20 5.00 3 3 -15 -3.30 4.50 -2 -3 15 -6.40 6.10 -2 -3 15 8.20 6.10 -2 -3 15 11.40 7.90 2 -3 -15 0.40 4.20 -2 -3 15 -0.70 7.50 -2 3 15 -3.20 5.70 2 3 -15 5.90 4.50 -2 3 15 1.00 7.00 -2 3 15 3.40 5.30 -2 3 15 2.90 8.30 -3 -4 15 4.00 5.30 -3 -4 15 3.90 5.50 -3 -4 15 -2.70 8.80 3 -4 -15 -0.20 3.90 -3 -4 15 1.30 7.70 -3 4 15 9.60 8.70 -3 4 15 -1.30 4.80 -3 4 15 -11.90 6.60 -3 4 15 -0.80 4.90 -2 -4 15 5.00 5.90 -2 -4 15 7.80 9.40 -2 -4 15 4.90 8.10 -2 -4 15 -3.40 6.10 2 -4 -15 -0.60 4.20 -2 4 15 8.70 7.30 2 4 -15 1.60 4.50 -2 4 15 -3.80 5.60 -2 4 15 3.40 5.40 -2 4 15 2.50 8.80 -3 -5 15 0.60 8.00 -3 -5 15 -6.70 7.70 -3 -5 15 2.20 5.30 -3 -5 15 -7.10 5.40 3 -5 -15 -5.30 3.80 -3 5 15 3.30 5.00 -3 5 15 -5.00 4.80 -3 5 15 -9.60 6.60 -3 5 15 -3.70 8.40 -2 -5 15 11.40 9.10 2 -5 -15 -1.00 4.10 -2 -5 15 1.70 5.50 -2 -5 15 2.90 8.00 -2 -5 15 3.90 6.30 -2 5 15 -2.40 7.10 -2 5 15 0.20 5.40 2 5 -15 -4.40 4.30 -2 5 15 1.30 5.70 -2 5 15 16.70 9.20 -3 -6 15 2.20 8.90 -3 -6 15 8.10 8.90 -3 -6 15 4.60 5.60 -3 6 15 23.80 9.70 -3 6 15 3.30 5.00 -2 -6 15 19.00 9.40 -2 -6 15 17.00 9.30 -2 -6 15 18.60 6.80 2 6 -15 11.00 5.00 -2 6 15 20.70 6.50 -2 6 15 30.70 6.50 -2 6 15 23.00 9.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 85103 _shelx_res_file ; TITL KH3_c.res in P2(1)/n shelx.res created by SHELXL-2019/3 at 20:09:06 on 25-Aug-2024 CELL 0.71073 8.2664 34.7886 12.5972 90.000 104.550 90.000 ZERR 4.00 0.0004 0.0018 0.0006 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S BR UNIT 144 108 12 24 12 8 MERG 2 OMIT 1 4 0 OMIT 3 1 3 FMAP 2 PLAN 20 SIZE 0.040 0.190 0.290 ACTA 50.00 BOND $H CONF EQIV $1 1/2+x,1/2-y,-1/2+z EQIV $2 1-x,1-y,1-z EQIV $3 1/2+X,1/2-Y,1/2+Z HTAB C19 O4_$1 HTAB C27 O1_$2 HTAB C2 O1 HTAB C15 O2 HTAB C22 O6 HTAB C29 O5 RTAB D2CG C35 C16_$3 C17_$3 C18_$3 C19_$3 C20_$3 C21_$3 RTAB D2CG H35 C16_$3 C17_$3 C18_$3 C19_$3 C20_$3 C21_$3 L.S. 30 WGHT 0.039700 5.098300 FVAR 0.29565 C1 1 0.226644 0.421121 0.611204 11.00000 0.04195 0.03837 = 0.05239 -0.00915 -0.00571 0.00289 C2 1 0.207464 0.458361 0.568802 11.00000 0.07827 0.04000 = 0.07056 0.00094 -0.01554 0.00752 AFIX 43 H2 2 0.242319 0.465117 0.506636 11.00000 -1.20000 AFIX 0 C3 1 0.134081 0.484559 0.624078 11.00000 0.09063 0.04438 = 0.10970 -0.02138 -0.02151 0.02323 AFIX 43 H3 2 0.119704 0.509708 0.598397 11.00000 -1.20000 AFIX 0 C4 1 0.081397 0.474994 0.715512 11.00000 0.05997 0.07270 = 0.11865 -0.05010 -0.01905 0.03104 AFIX 43 H4 2 0.032049 0.493682 0.749854 11.00000 -1.20000 AFIX 0 C5 1 0.100165 0.438163 0.757609 11.00000 0.04475 0.08271 = 0.07646 -0.03112 0.00392 0.01656 AFIX 43 H5 2 0.065741 0.431822 0.820239 11.00000 -1.20000 AFIX 0 C6 1 0.172631 0.410752 0.702901 11.00000 0.03246 0.05498 = 0.05172 -0.01701 0.00051 0.00937 C7 1 0.217950 0.371171 0.723922 11.00000 0.03576 0.05358 = 0.03847 -0.00041 0.00578 0.00439 C8 1 0.298625 0.358084 0.650612 11.00000 0.03572 0.03594 = 0.03530 0.00126 0.00615 0.00203 C9 1 0.054207 0.374953 0.392894 11.00000 0.05050 0.04595 = 0.03296 -0.00476 0.01083 0.00195 C10 1 -0.044078 0.406001 0.348819 11.00000 0.06658 0.05842 = 0.04039 0.00270 0.00409 0.00650 AFIX 43 H10 2 0.004062 0.429860 0.343575 11.00000 -1.20000 AFIX 0 C11 1 -0.214672 0.401087 0.312704 11.00000 0.07075 0.09098 = 0.04435 -0.00548 0.00009 0.02542 AFIX 43 H11 2 -0.282247 0.421807 0.283294 11.00000 -1.20000 AFIX 0 C12 1 -0.284441 0.366175 0.319858 11.00000 0.05162 0.11067 = 0.05783 -0.02683 0.00658 0.00143 AFIX 43 H12 2 -0.399556 0.363131 0.295081 11.00000 -1.20000 AFIX 0 C13 1 -0.186547 0.335305 0.363363 11.00000 0.06537 0.08006 = 0.06829 -0.02381 0.01777 -0.02405 AFIX 43 H13 2 -0.235668 0.311493 0.367608 11.00000 -1.20000 AFIX 0 C14 1 -0.015788 0.339438 0.400781 11.00000 0.06562 0.04820 = 0.05182 -0.00832 0.00823 -0.00382 AFIX 43 H14 2 0.050914 0.318655 0.430778 11.00000 -1.20000 AFIX 0 C15 1 0.393822 0.321257 0.648880 11.00000 0.04638 0.03111 = 0.04560 -0.00129 0.00858 0.00518 AFIX 23 H15A 2 0.315178 0.300654 0.621888 11.00000 -1.20000 H15B 2 0.464582 0.324063 0.598503 11.00000 -1.20000 AFIX 0 C16 1 0.641473 0.246959 0.695911 11.00000 0.05316 0.02880 = 0.04549 -0.00003 0.01031 0.00681 C17 1 0.809873 0.240446 0.741484 11.00000 0.05061 0.07141 = 0.06083 -0.01376 0.00864 0.00746 AFIX 43 H17 2 0.853833 0.242415 0.816857 11.00000 -1.20000 AFIX 0 C18 1 0.911729 0.231003 0.673846 11.00000 0.05711 0.09217 = 0.11626 -0.02085 0.03013 0.00757 AFIX 43 H18 2 1.024933 0.226412 0.703439 11.00000 -1.20000 AFIX 0 C19 1 0.845404 0.228418 0.562881 11.00000 0.13387 0.07028 = 0.09313 0.00267 0.07473 0.01766 AFIX 43 H19 2 0.914182 0.222430 0.517049 11.00000 -1.20000 AFIX 0 C20 1 0.678552 0.234602 0.519219 11.00000 0.15199 0.08274 = 0.04943 -0.00207 0.02935 0.05758 AFIX 43 H20 2 0.634731 0.232593 0.443842 11.00000 -1.20000 AFIX 0 C21 1 0.575602 0.243676 0.584796 11.00000 0.08948 0.05140 = 0.05399 -0.01049 0.00607 0.02469 AFIX 43 H21 2 0.462055 0.247598 0.554608 11.00000 -1.20000 AFIX 0 C22 1 0.662768 0.330725 0.793841 11.00000 0.03924 0.04560 = 0.04978 -0.01035 0.00759 0.00045 AFIX 23 H22A 2 0.717555 0.322827 0.868007 11.00000 -1.20000 H22B 2 0.732885 0.322749 0.746573 11.00000 -1.20000 AFIX 0 C23 1 0.648881 0.373304 0.790654 11.00000 0.03423 0.04374 = 0.03762 -0.00919 0.00622 -0.00231 C24 1 0.681629 0.397174 0.714342 11.00000 0.03806 0.05932 = 0.04074 -0.00823 0.01339 -0.01377 C25 1 0.642149 0.435929 0.736845 11.00000 0.04174 0.04948 = 0.04463 -0.00156 0.00547 -0.01511 C26 1 0.645139 0.470795 0.681157 11.00000 0.06123 0.06789 = 0.06261 0.01504 0.01152 -0.02111 AFIX 43 H26 2 0.682286 0.471908 0.617395 11.00000 -1.20000 AFIX 0 C27 1 0.591157 0.503201 0.724354 11.00000 0.07748 0.04704 = 0.08679 0.01904 -0.00276 -0.01377 AFIX 43 H27 2 0.592151 0.526653 0.689090 11.00000 -1.20000 AFIX 0 C28 1 0.535773 0.501795 0.818339 11.00000 0.07661 0.03923 = 0.08933 -0.00008 0.00872 -0.00075 AFIX 43 H28 2 0.501929 0.524470 0.845424 11.00000 -1.20000 AFIX 0 C29 1 0.528632 0.468286 0.873434 11.00000 0.05514 0.04508 = 0.05665 -0.00743 0.00397 0.00289 AFIX 43 H29 2 0.487987 0.467571 0.935870 11.00000 -1.20000 AFIX 0 C30 1 0.585377 0.435061 0.831500 11.00000 0.04157 0.03487 = 0.04346 -0.00161 0.00210 -0.00410 C31 1 0.848227 0.391727 1.048005 11.00000 0.04271 0.05888 = 0.03146 -0.00733 0.00965 -0.00409 C32 1 0.912194 0.428494 1.051366 11.00000 0.05790 0.08333 = 0.06037 0.00682 -0.00030 -0.01784 AFIX 43 H32 2 0.841943 0.449515 1.030325 11.00000 -1.20000 AFIX 0 C33 1 1.083803 0.433276 1.086903 11.00000 0.07222 0.13240 = 0.07004 0.00684 0.00362 -0.05296 AFIX 43 H33 2 1.130676 0.457639 1.088526 11.00000 -1.20000 AFIX 0 C34 1 1.184275 0.401751 1.119745 11.00000 0.04217 0.19626 = 0.05809 -0.01844 0.01861 -0.00784 AFIX 43 H34 2 1.299428 0.405079 1.142745 11.00000 -1.20000 AFIX 0 C35 1 1.119022 0.365674 1.119398 11.00000 0.05273 0.13418 = 0.07291 -0.03311 0.00207 0.02839 AFIX 43 H35 2 1.188587 0.344814 1.144262 11.00000 -1.20000 AFIX 0 C36 1 0.947872 0.360500 1.081552 11.00000 0.05969 0.07391 = 0.06125 -0.01975 0.00706 0.01280 AFIX 43 H36 2 0.901555 0.336052 1.079059 11.00000 -1.20000 AFIX 0 N1 3 0.305374 0.388628 0.576024 11.00000 0.04509 0.03492 = 0.03853 -0.00039 0.00790 0.00241 N2 3 0.498996 0.310639 0.758767 11.00000 0.04160 0.03093 = 0.04412 0.00295 0.01057 0.00464 N3 3 0.587852 0.396052 0.866861 11.00000 0.04155 0.03605 = 0.03480 -0.00329 0.00946 -0.00126 O1 4 0.321403 0.414884 0.395799 11.00000 0.08316 0.07182 = 0.06317 0.02015 0.01826 -0.01963 O2 4 0.352105 0.345144 0.427261 11.00000 0.05843 0.06836 = 0.04650 -0.00846 0.01955 0.00972 O3 4 0.352345 0.248006 0.743012 11.00000 0.05817 0.04823 = 0.11835 0.01290 0.03400 -0.00671 O4 4 0.607109 0.258305 0.892238 11.00000 0.09929 0.05748 = 0.04519 0.01429 0.02602 0.02211 O5 4 0.547485 0.413141 1.049473 11.00000 0.05430 0.06987 = 0.04607 -0.00749 0.02282 0.00562 O6 4 0.594833 0.345483 1.009178 11.00000 0.07387 0.05158 = 0.05619 0.00626 0.01624 -0.01819 S1 5 0.272429 0.380603 0.439934 11.00000 0.05284 0.05147 = 0.03650 0.00500 0.01260 -0.00418 S2 5 0.515533 0.263646 0.780554 11.00000 0.05409 0.03572 = 0.05508 0.00760 0.02113 0.00616 S3 5 0.630834 0.385128 1.001216 11.00000 0.04163 0.04733 = 0.03777 -0.00272 0.01361 -0.00500 BR1 6 0.747769 0.382496 0.589528 11.00000 0.06607 0.10847 = 0.05354 -0.02468 0.03331 -0.02725 BR2 6 0.173440 0.344267 0.841365 11.00000 0.06881 0.11270 = 0.06103 0.02248 0.03524 0.01274 HKLF 4 REM KH3_c.res in P2(1)/n REM wR2 = 0.1199, GooF = S = 1.118, Restrained GooF = 1.118 for all data REM R1 = 0.0478 for 5196 Fo > 4sig(Fo) and 0.0621 for all 6434 data REM 451 parameters refined using 0 restraints END WGHT 0.0398 5.0924 REM Highest difference peak 0.458, deepest hole -0.466, 1-sigma level 0.065 Q1 1 0.6925 0.3805 0.6475 11.00000 0.05 0.46 Q2 1 0.0979 0.3464 0.8780 11.00000 0.05 0.44 Q3 1 0.8286 0.3723 0.5517 11.00000 0.05 0.40 Q4 1 0.5926 0.2551 0.7400 11.00000 0.05 0.36 Q5 1 0.1355 0.3319 0.7768 11.00000 0.05 0.35 Q6 1 0.2563 0.3481 0.8024 11.00000 0.05 0.34 Q7 1 0.2288 0.3489 0.7763 11.00000 0.05 0.33 Q8 1 0.7500 0.3882 1.0038 11.00000 0.05 0.31 Q9 1 0.5623 0.3932 1.0391 11.00000 0.05 0.28 Q10 1 0.1622 0.3784 0.4121 11.00000 0.05 0.27 Q11 1 0.7060 0.2644 0.8625 11.00000 0.05 0.27 Q12 1 0.2212 0.3243 0.8769 11.00000 0.05 0.25 Q13 1 0.6577 0.3881 0.9256 11.00000 0.05 0.25 Q14 1 0.7986 0.3487 0.6077 11.00000 0.05 0.24 Q15 1 0.6306 0.4656 0.6030 11.00000 0.05 0.22 Q16 1 0.2342 0.4310 0.4062 11.00000 0.05 0.22 Q17 1 0.0153 0.4787 0.7812 11.00000 0.05 0.22 Q18 1 0.2389 0.3801 0.5213 11.00000 0.05 0.21 Q19 1 0.9113 0.3673 0.6012 11.00000 0.05 0.21 Q20 1 0.3394 0.3933 0.4002 11.00000 0.05 0.21 ; _shelx_res_checksum 2149 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.2266(5) 0.42112(11) 0.6112(3) 0.0474(10) Uani d 1 . . C C2 0.2075(6) 0.45836(12) 0.5688(4) 0.0691(14) Uani d 1 . . H H2 0.242319 0.465117 0.506636 0.083 Uiso calc 1 . . C C3 0.1341(8) 0.48456(15) 0.6241(6) 0.090(2) Uani d 1 . . H H3 0.119704 0.509708 0.598397 0.108 Uiso calc 1 . . C C4 0.0814(7) 0.47499(17) 0.7155(6) 0.091(2) Uani d 1 . . H H4 0.032049 0.493682 0.749854 0.109 Uiso calc 1 . . C C5 0.1002(5) 0.43816(16) 0.7576(4) 0.0700(14) Uani d 1 . . H H5 0.065741 0.431822 0.820239 0.084 Uiso calc 1 . . C C6 0.1726(5) 0.41075(12) 0.7029(3) 0.0482(10) Uani d 1 . . C C7 0.2180(5) 0.37117(11) 0.7239(3) 0.0432(9) Uani d 1 . . C C8 0.2986(4) 0.35808(10) 0.6506(3) 0.0361(8) Uani d 1 . . C C9 0.0542(5) 0.37495(11) 0.3929(3) 0.0431(9) Uani d 1 . . C C10 -0.0441(6) 0.40600(13) 0.3488(3) 0.0568(11) Uani d 1 . . H H10 0.004062 0.429860 0.343575 0.068 Uiso calc 1 . . C C11 -0.2147(7) 0.40109(18) 0.3127(4) 0.0713(14) Uani d 1 . . H H11 -0.282247 0.421807 0.283294 0.086 Uiso calc 1 . . C C12 -0.2844(6) 0.36617(19) 0.3199(4) 0.0747(15) Uani d 1 . . H H12 -0.399556 0.363131 0.295081 0.090 Uiso calc 1 . . C C13 -0.1865(6) 0.33531(16) 0.3634(4) 0.0711(14) Uani d 1 . . H H13 -0.235668 0.311493 0.367608 0.085 Uiso calc 1 . . C C14 -0.0158(6) 0.33944(12) 0.4008(4) 0.0564(11) Uani d 1 . . H H14 0.050914 0.318655 0.430778 0.068 Uiso calc 1 . . C C15 0.3938(5) 0.32126(10) 0.6489(3) 0.0416(9) Uani d 1 . . H H15A 0.315178 0.300654 0.621888 0.050 Uiso calc 1 . . H H15B 0.464582 0.324063 0.598503 0.050 Uiso calc 1 . . C C16 0.6415(5) 0.24696(10) 0.6959(3) 0.0429(9) Uani d 1 . . C C17 0.8099(6) 0.24045(14) 0.7415(4) 0.0619(12) Uani d 1 . . H H17 0.853833 0.242415 0.816857 0.074 Uiso calc 1 . . C C18 0.9117(7) 0.23100(17) 0.6738(6) 0.0870(18) Uani d 1 . . H H18 1.024933 0.226412 0.703439 0.104 Uiso calc 1 . . C C19 0.8454(10) 0.22842(16) 0.5629(6) 0.091(2) Uani d 1 . . H H19 0.914182 0.222430 0.517049 0.109 Uiso calc 1 . . C C20 0.6786(10) 0.23460(17) 0.5192(4) 0.094(2) Uani d 1 . . H H20 0.634731 0.232593 0.443842 0.113 Uiso calc 1 . . C C21 0.5756(7) 0.24368(13) 0.5848(4) 0.0671(14) Uani d 1 . . H H21 0.462055 0.247598 0.554608 0.081 Uiso calc 1 . . C C22 0.6628(5) 0.33072(11) 0.7938(3) 0.0455(9) Uani d 1 . . H H22A 0.717555 0.322827 0.868007 0.055 Uiso calc 1 . . H H22B 0.732885 0.322749 0.746573 0.055 Uiso calc 1 . . C C23 0.6489(4) 0.37330(11) 0.7907(3) 0.0390(8) Uani d 1 . . C C24 0.6816(5) 0.39717(12) 0.7143(3) 0.0454(9) Uani d 1 . . C C25 0.6421(5) 0.43593(12) 0.7368(3) 0.0462(9) Uani d 1 . . C C26 0.6451(6) 0.47079(14) 0.6812(4) 0.0646(13) Uani d 1 . . H H26 0.682286 0.471908 0.617395 0.078 Uiso calc 1 . . C C27 0.5912(7) 0.50320(14) 0.7244(5) 0.0746(15) Uani d 1 . . H H27 0.592151 0.526653 0.689090 0.090 Uiso calc 1 . . C C28 0.5358(7) 0.50180(13) 0.8183(5) 0.0706(14) Uani d 1 . . H H28 0.501929 0.524470 0.845424 0.085 Uiso calc 1 . . C C29 0.5286(5) 0.46829(12) 0.8734(4) 0.0541(11) Uani d 1 . . H H29 0.487987 0.467571 0.935870 0.065 Uiso calc 1 . . C C30 0.5854(5) 0.43506(10) 0.8315(3) 0.0415(9) Uani d 1 . . C C31 0.8482(5) 0.39173(12) 1.0480(3) 0.0443(9) Uani d 1 . . C C32 0.9122(6) 0.42849(16) 1.0514(4) 0.0699(14) Uani d 1 . . H H32 0.841943 0.449515 1.030325 0.084 Uiso calc 1 . . C C33 1.0838(8) 0.4333(2) 1.0869(5) 0.094(2) Uani d 1 . . H H33 1.130676 0.457639 1.088526 0.113 Uiso calc 1 . . C C34 1.1843(7) 0.4018(3) 1.1197(5) 0.098(2) Uani d 1 . . H H34 1.299428 0.405079 1.142745 0.117 Uiso calc 1 . . C C35 1.1190(7) 0.3657(2) 1.1194(5) 0.0891(19) Uani d 1 . . H H35 1.188587 0.344814 1.144262 0.107 Uiso calc 1 . . C C36 0.9479(6) 0.36050(15) 1.0816(4) 0.0664(13) Uani d 1 . . H H36 0.901555 0.336052 1.079059 0.080 Uiso calc 1 . . N N1 0.3054(4) 0.38863(8) 0.5760(2) 0.0400(7) Uani d 1 . . N N2 0.4990(4) 0.31064(8) 0.7588(2) 0.0389(7) Uani d 1 . . N N3 0.5879(4) 0.39605(8) 0.8669(2) 0.0375(7) Uani d 1 . . O O1 0.3214(4) 0.41488(10) 0.3958(3) 0.0727(9) Uani d 1 . . O O2 0.3521(4) 0.34514(9) 0.4273(2) 0.0566(7) Uani d 1 . . O O3 0.3523(4) 0.24801(9) 0.7430(3) 0.0728(10) Uani d 1 . . O O4 0.6071(5) 0.25830(9) 0.8922(2) 0.0659(9) Uani d 1 . . O O5 0.5475(4) 0.41314(9) 1.0495(2) 0.0549(7) Uani d 1 . . O O6 0.5948(4) 0.34548(8) 1.0092(2) 0.0606(8) Uani d 1 . . S S1 0.27243(13) 0.38060(3) 0.43993(8) 0.0467(2) Uani d 1 . . S S2 0.51553(13) 0.26365(3) 0.78055(9) 0.0470(2) Uani d 1 . . S S3 0.63083(12) 0.38513(3) 1.00122(8) 0.0416(2) Uani d 1 . . Br Br1 0.74777(6) 0.38250(2) 0.58953(4) 0.07276(18) Uani d 1 . . Br Br2 0.17344(7) 0.34427(2) 0.84137(4) 0.07746(19) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.042(2) 0.038(2) 0.052(2) 0.0029(17) -0.0057(18) -0.0091(18) C2 0.078(3) 0.040(2) 0.071(3) 0.008(2) -0.016(3) 0.001(2) C3 0.091(4) 0.044(3) 0.110(5) 0.023(3) -0.022(4) -0.021(3) C4 0.060(3) 0.073(4) 0.119(5) 0.031(3) -0.019(3) -0.050(4) C5 0.045(3) 0.083(4) 0.076(3) 0.017(2) 0.004(2) -0.031(3) C6 0.0325(19) 0.055(2) 0.052(2) 0.0094(17) 0.0005(17) -0.0170(19) C7 0.036(2) 0.054(2) 0.038(2) 0.0044(17) 0.0058(16) -0.0004(17) C8 0.0357(19) 0.0359(19) 0.0353(19) 0.0020(15) 0.0061(15) 0.0013(15) C9 0.051(2) 0.046(2) 0.0330(19) 0.0019(18) 0.0108(17) -0.0048(16) C10 0.067(3) 0.058(3) 0.040(2) 0.007(2) 0.004(2) 0.0027(19) C11 0.071(3) 0.091(4) 0.044(3) 0.025(3) 0.000(2) -0.005(2) C12 0.052(3) 0.111(5) 0.058(3) 0.001(3) 0.007(2) -0.027(3) C13 0.065(3) 0.080(4) 0.068(3) -0.024(3) 0.018(3) -0.024(3) C14 0.066(3) 0.048(2) 0.052(3) -0.004(2) 0.008(2) -0.0083(19) C15 0.046(2) 0.0311(19) 0.046(2) 0.0052(16) 0.0086(17) -0.0013(16) C16 0.053(2) 0.0288(19) 0.045(2) 0.0068(16) 0.0103(18) 0.0000(16) C17 0.051(3) 0.071(3) 0.061(3) 0.007(2) 0.009(2) -0.014(2) C18 0.057(3) 0.092(4) 0.116(5) 0.008(3) 0.030(3) -0.021(4) C19 0.134(6) 0.070(4) 0.093(5) 0.018(4) 0.075(4) 0.003(3) C20 0.152(6) 0.083(4) 0.049(3) 0.058(4) 0.029(3) -0.002(3) C21 0.089(4) 0.051(3) 0.054(3) 0.025(2) 0.006(3) -0.010(2) C22 0.039(2) 0.046(2) 0.050(2) 0.0004(17) 0.0076(17) -0.0103(18) C23 0.0342(19) 0.044(2) 0.0376(19) -0.0023(15) 0.0062(15) -0.0092(16) C24 0.038(2) 0.059(3) 0.041(2) -0.0138(18) 0.0134(17) -0.0082(18) C25 0.042(2) 0.049(2) 0.045(2) -0.0151(18) 0.0055(18) -0.0016(18) C26 0.061(3) 0.068(3) 0.063(3) -0.021(2) 0.012(2) 0.015(2) C27 0.077(3) 0.047(3) 0.087(4) -0.014(2) -0.003(3) 0.019(3) C28 0.077(3) 0.039(3) 0.089(4) -0.001(2) 0.009(3) 0.000(2) C29 0.055(3) 0.045(2) 0.057(3) 0.0029(19) 0.004(2) -0.007(2) C30 0.042(2) 0.035(2) 0.043(2) -0.0041(16) 0.0021(17) -0.0016(16) C31 0.043(2) 0.059(3) 0.0315(19) -0.0041(18) 0.0097(16) -0.0073(17) C32 0.058(3) 0.083(4) 0.060(3) -0.018(3) 0.000(2) 0.007(3) C33 0.072(4) 0.132(6) 0.070(4) -0.053(4) 0.004(3) 0.007(4) C34 0.042(3) 0.196(8) 0.058(3) -0.008(4) 0.019(3) -0.018(4) C35 0.053(3) 0.134(6) 0.073(4) 0.028(4) 0.002(3) -0.033(4) C36 0.060(3) 0.074(3) 0.061(3) 0.013(2) 0.007(2) -0.020(2) N1 0.0451(17) 0.0349(16) 0.0385(17) 0.0024(13) 0.0079(14) -0.0004(13) N2 0.0416(17) 0.0309(16) 0.0441(17) 0.0046(13) 0.0106(14) 0.0029(13) N3 0.0416(17) 0.0360(16) 0.0348(16) -0.0013(13) 0.0095(13) -0.0033(12) O1 0.083(2) 0.072(2) 0.063(2) -0.0196(18) 0.0183(18) 0.0201(17) O2 0.0584(18) 0.068(2) 0.0465(16) 0.0097(15) 0.0196(14) -0.0085(14) O3 0.0582(19) 0.0482(18) 0.118(3) -0.0067(15) 0.034(2) 0.0129(18) O4 0.099(3) 0.0575(19) 0.0452(17) 0.0221(17) 0.0260(17) 0.0143(14) O5 0.0543(17) 0.0699(19) 0.0461(16) 0.0056(14) 0.0228(14) -0.0075(14) O6 0.074(2) 0.0516(18) 0.0562(18) -0.0182(15) 0.0162(16) 0.0063(14) S1 0.0528(6) 0.0515(6) 0.0365(5) -0.0042(5) 0.0126(4) 0.0050(4) S2 0.0541(6) 0.0357(5) 0.0551(6) 0.0062(4) 0.0211(5) 0.0076(4) S3 0.0416(5) 0.0473(5) 0.0378(5) -0.0050(4) 0.0136(4) -0.0027(4) Br1 0.0661(3) 0.1085(4) 0.0535(3) -0.0273(3) 0.0333(2) -0.0247(3) Br2 0.0688(3) 0.1127(5) 0.0610(3) 0.0127(3) 0.0352(3) 0.0225(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C6 C1 C2 . . 122.1(4) ? C6 C1 N1 . . 108.6(3) ? C2 C1 N1 . . 129.2(4) ? C3 C2 C1 . . 116.3(6) ? C3 C2 H2 . . 121.8 ? C1 C2 H2 . . 121.8 ? C4 C3 C2 . . 122.5(5) ? C4 C3 H3 . . 118.7 ? C2 C3 H3 . . 118.7 ? C3 C4 C5 . . 121.3(5) ? C3 C4 H4 . . 119.4 ? C5 C4 H4 . . 119.4 ? C4 C5 C6 . . 117.7(6) ? C4 C5 H5 . . 121.1 ? C6 C5 H5 . . 121.1 ? C1 C6 C5 . . 120.1(4) ? C1 C6 C7 . . 106.2(3) ? C5 C6 C7 . . 133.6(5) ? C8 C7 C6 . . 110.4(4) ? C8 C7 Br2 . . 127.2(3) ? C6 C7 Br2 . . 122.3(3) ? C7 C8 N1 . . 107.9(3) ? C7 C8 C15 . . 130.4(3) ? N1 C8 C15 . . 121.1(3) ? C14 C9 C10 . . 121.0(4) ? C14 C9 S1 . . 119.2(3) ? C10 C9 S1 . . 119.8(3) ? C11 C10 C9 . . 119.0(5) ? C11 C10 H10 . . 120.5 ? C9 C10 H10 . . 120.5 ? C12 C11 C10 . . 120.4(5) ? C12 C11 H11 . . 119.8 ? C10 C11 H11 . . 119.8 ? C11 C12 C13 . . 120.6(5) ? C11 C12 H12 . . 119.7 ? C13 C12 H12 . . 119.7 ? C12 C13 C14 . . 120.3(5) ? C12 C13 H13 . . 119.8 ? C14 C13 H13 . . 119.8 ? C9 C14 C13 . . 118.8(4) ? C9 C14 H14 . . 120.6 ? C13 C14 H14 . . 120.6 ? N2 C15 C8 . . 112.6(3) ? N2 C15 H15A . . 109.1 ? C8 C15 H15A . . 109.1 ? N2 C15 H15B . . 109.1 ? C8 C15 H15B . . 109.1 ? H15A C15 H15B . . 107.8 ? C21 C16 C17 . . 120.6(4) ? C21 C16 S2 . . 120.0(3) ? C17 C16 S2 . . 119.2(3) ? C18 C17 C16 . . 119.3(5) ? C18 C17 H17 . . 120.4 ? C16 C17 H17 . . 120.4 ? C19 C18 C17 . . 119.7(5) ? C19 C18 H18 . . 120.1 ? C17 C18 H18 . . 120.1 ? C20 C19 C18 . . 120.3(5) ? C20 C19 H19 . . 119.8 ? C18 C19 H19 . . 119.8 ? C21 C20 C19 . . 120.8(5) ? C21 C20 H20 . . 119.6 ? C19 C20 H20 . . 119.6 ? C20 C21 C16 . . 119.3(5) ? C20 C21 H21 . . 120.4 ? C16 C21 H21 . . 120.4 ? C23 C22 N2 . . 113.7(3) ? C23 C22 H22A . . 108.8 ? N2 C22 H22A . . 108.8 ? C23 C22 H22B . . 108.8 ? N2 C22 H22B . . 108.8 ? H22A C22 H22B . . 107.7 ? C24 C23 N3 . . 107.8(3) ? C24 C23 C22 . . 127.3(3) ? N3 C23 C22 . . 124.9(3) ? C23 C24 C25 . . 110.0(3) ? C23 C24 Br1 . . 126.0(3) ? C25 C24 Br1 . . 123.7(3) ? C30 C25 C26 . . 120.0(4) ? C30 C25 C24 . . 107.0(3) ? C26 C25 C24 . . 132.9(4) ? C27 C26 C25 . . 117.5(5) ? C27 C26 H26 . . 121.2 ? C25 C26 H26 . . 121.2 ? C28 C27 C26 . . 121.6(5) ? C28 C27 H27 . . 119.2 ? C26 C27 H27 . . 119.2 ? C29 C28 C27 . . 122.3(5) ? C29 C28 H28 . . 118.8 ? C27 C28 H28 . . 118.8 ? C28 C29 C30 . . 116.9(5) ? C28 C29 H29 . . 121.6 ? C30 C29 H29 . . 121.6 ? C25 C30 C29 . . 121.6(4) ? C25 C30 N3 . . 107.9(3) ? C29 C30 N3 . . 130.3(4) ? C36 C31 C32 . . 122.1(4) ? C36 C31 S3 . . 119.1(3) ? C32 C31 S3 . . 118.8(3) ? C31 C32 C33 . . 118.3(5) ? C31 C32 H32 . . 120.9 ? C33 C32 H32 . . 120.9 ? C34 C33 C32 . . 119.6(6) ? C34 C33 H33 . . 120.2 ? C32 C33 H33 . . 120.2 ? C35 C34 C33 . . 121.6(5) ? C35 C34 H34 . . 119.2 ? C33 C34 H34 . . 119.2 ? C34 C35 C36 . . 119.2(6) ? C34 C35 H35 . . 120.4 ? C36 C35 H35 . . 120.4 ? C31 C36 C35 . . 119.2(5) ? C31 C36 H36 . . 120.4 ? C35 C36 H36 . . 120.4 ? C8 N1 C1 . . 106.8(3) ? C8 N1 S1 . . 121.4(2) ? C1 N1 S1 . . 118.4(3) ? C15 N2 C22 . . 115.8(3) ? C15 N2 S2 . . 113.9(2) ? C22 N2 S2 . . 112.5(2) ? C30 N3 C23 . . 107.2(3) ? C30 N3 S3 . . 120.8(2) ? C23 N3 S3 . . 121.9(2) ? O1 S1 O2 . . 119.9(2) ? O1 S1 N1 . . 105.65(19) ? O2 S1 N1 . . 107.17(16) ? O1 S1 C9 . . 109.3(2) ? O2 S1 C9 . . 109.17(18) ? N1 S1 C9 . . 104.47(17) ? O3 S2 O4 . . 120.0(2) ? O3 S2 N2 . . 106.90(17) ? O4 S2 N2 . . 106.97(18) ? O3 S2 C16 . . 109.1(2) ? O4 S2 C16 . . 107.72(19) ? N2 S2 C16 . . 105.13(17) ? O5 S3 O6 . . 120.34(19) ? O5 S3 N3 . . 105.89(16) ? O6 S3 N3 . . 107.18(17) ? O5 S3 C31 . . 109.42(18) ? O6 S3 C31 . . 108.5(2) ? N3 S3 C31 . . 104.31(17) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C6 . 1.387(6) ? C1 C2 . 1.395(6) ? C1 N1 . 1.429(5) ? C2 C3 . 1.377(8) ? C2 H2 . 0.9300 ? C3 C4 . 1.371(9) ? C3 H3 . 0.9300 ? C4 C5 . 1.380(8) ? C4 H4 . 0.9300 ? C5 C6 . 1.397(6) ? C5 H5 . 0.9300 ? C6 C7 . 1.434(6) ? C7 C8 . 1.347(5) ? C7 Br2 . 1.864(4) ? C8 N1 . 1.429(5) ? C8 C15 . 1.507(5) ? C9 C14 . 1.378(6) ? C9 C10 . 1.381(6) ? C9 S1 . 1.763(4) ? C10 C11 . 1.379(7) ? C10 H10 . 0.9300 ? C11 C12 . 1.357(8) ? C11 H11 . 0.9300 ? C12 C13 . 1.373(8) ? C12 H12 . 0.9300 ? C13 C14 . 1.379(7) ? C13 H13 . 0.9300 ? C14 H14 . 0.9300 ? C15 N2 . 1.485(5) ? C15 H15A . 0.9700 ? C15 H15B . 0.9700 ? C16 C21 . 1.373(6) ? C16 C17 . 1.385(6) ? C16 S2 . 1.765(4) ? C17 C18 . 1.380(7) ? C17 H17 . 0.9300 ? C18 C19 . 1.370(9) ? C18 H18 . 0.9300 ? C19 C20 . 1.367(9) ? C19 H19 . 0.9300 ? C20 C21 . 1.364(8) ? C20 H20 . 0.9300 ? C21 H21 . 0.9300 ? C22 C23 . 1.485(5) ? C22 N2 . 1.489(5) ? C22 H22A . 0.9700 ? C22 H22B . 0.9700 ? C23 C24 . 1.348(5) ? C23 N3 . 1.430(4) ? C24 C25 . 1.432(6) ? C24 Br1 . 1.861(4) ? C25 C30 . 1.387(6) ? C25 C26 . 1.405(6) ? C26 C27 . 1.374(7) ? C26 H26 . 0.9300 ? C27 C28 . 1.373(8) ? C27 H27 . 0.9300 ? C28 C29 . 1.366(6) ? C28 H28 . 0.9300 ? C29 C30 . 1.400(6) ? C29 H29 . 0.9300 ? C30 N3 . 1.427(5) ? C31 C36 . 1.365(6) ? C31 C32 . 1.381(6) ? C31 S3 . 1.760(4) ? C32 C33 . 1.386(7) ? C32 H32 . 0.9300 ? C33 C34 . 1.375(10) ? C33 H33 . 0.9300 ? C34 C35 . 1.366(10) ? C34 H34 . 0.9300 ? C35 C36 . 1.387(7) ? C35 H35 . 0.9300 ? C36 H36 . 0.9300 ? N1 S1 . 1.690(3) ? N2 S2 . 1.658(3) ? N3 S3 . 1.683(3) ? O1 S1 . 1.417(3) ? O2 S1 . 1.426(3) ? O3 S2 . 1.421(3) ? O4 S2 . 1.432(3) ? O5 S3 . 1.416(3) ? O6 S3 . 1.420(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C2 H2 O1 . 0.93 2.43 2.993(7) 119 yes C13 H13 O3 4_565 0.93 2.80 3.324(6) 117 yes C14 H14 O4 4_565 0.93 2.78 3.558(5) 142 yes C15 H15B O2 . 0.97 2.25 2.850(5) 119 yes C18 H18 O3 1_655 0.93 2.73 3.575(6) 151 yes C19 H19 O4 4_665 0.93 2.59 3.443(6) 152 yes C19 H19 O6 4_665 0.93 2.81 3.467(6) 129 yes C20 H20 Br2 4_665 0.93 3.02 3.536(5) 117 yes C22 H22A O6 . 0.97 2.39 2.950(5) 116 yes C27 H27 O1 3_666 0.93 2.48 3.389(6) 164 yes C28 H28 O5 3_667 0.93 2.63 3.547(6) 170 yes C29 H29 O5 . 0.93 2.35 2.907(5) 118 yes C34 H34 O5 1_655 0.93 2.62 3.360(6) 137 yes C35 H35 Cg(C16--C21) 4_555 0.93 2.91 3.729(7) 147 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 1.0(6) ? N1 C1 C2 C3 . . . . -176.3(4) ? C1 C2 C3 C4 . . . . -0.3(8) ? C2 C3 C4 C5 . . . . 0.3(9) ? C3 C4 C5 C6 . . . . -0.9(8) ? C2 C1 C6 C5 . . . . -1.7(6) ? N1 C1 C6 C5 . . . . 176.1(3) ? C2 C1 C6 C7 . . . . -178.1(4) ? N1 C1 C6 C7 . . . . -0.4(4) ? C4 C5 C6 C1 . . . . 1.6(6) ? C4 C5 C6 C7 . . . . 176.9(4) ? C1 C6 C7 C8 . . . . 1.2(4) ? C5 C6 C7 C8 . . . . -174.6(4) ? C1 C6 C7 Br2 . . . . 179.2(3) ? C5 C6 C7 Br2 . . . . 3.4(6) ? C6 C7 C8 N1 . . . . -1.6(4) ? Br2 C7 C8 N1 . . . . -179.4(3) ? C6 C7 C8 C15 . . . . 169.0(4) ? Br2 C7 C8 C15 . . . . -8.8(6) ? C14 C9 C10 C11 . . . . 0.2(6) ? S1 C9 C10 C11 . . . . -179.8(3) ? C9 C10 C11 C12 . . . . -0.4(7) ? C10 C11 C12 C13 . . . . 0.2(8) ? C11 C12 C13 C14 . . . . 0.2(8) ? C10 C9 C14 C13 . . . . 0.2(6) ? S1 C9 C14 C13 . . . . -179.8(3) ? C12 C13 C14 C9 . . . . -0.5(7) ? C7 C8 C15 N2 . . . . -41.2(5) ? N1 C8 C15 N2 . . . . 128.3(3) ? C21 C16 C17 C18 . . . . 0.7(7) ? S2 C16 C17 C18 . . . . -173.8(4) ? C16 C17 C18 C19 . . . . 0.4(8) ? C17 C18 C19 C20 . . . . -1.0(9) ? C18 C19 C20 C21 . . . . 0.5(10) ? C19 C20 C21 C16 . . . . 0.6(9) ? C17 C16 C21 C20 . . . . -1.2(7) ? S2 C16 C21 C20 . . . . 173.2(4) ? N2 C22 C23 C24 . . . . -103.1(4) ? N2 C22 C23 N3 . . . . 73.1(5) ? N3 C23 C24 C25 . . . . -0.6(4) ? C22 C23 C24 C25 . . . . 176.1(3) ? N3 C23 C24 Br1 . . . . -174.8(3) ? C22 C23 C24 Br1 . . . . 1.9(6) ? C23 C24 C25 C30 . . . . 0.7(4) ? Br1 C24 C25 C30 . . . . 175.1(3) ? C23 C24 C25 C26 . . . . -176.4(4) ? Br1 C24 C25 C26 . . . . -2.0(6) ? C30 C25 C26 C27 . . . . 0.3(6) ? C24 C25 C26 C27 . . . . 177.2(4) ? C25 C26 C27 C28 . . . . -0.1(7) ? C26 C27 C28 C29 . . . . -1.0(8) ? C27 C28 C29 C30 . . . . 1.8(7) ? C26 C25 C30 C29 . . . . 0.6(6) ? C24 C25 C30 C29 . . . . -177.0(4) ? C26 C25 C30 N3 . . . . 177.0(3) ? C24 C25 C30 N3 . . . . -0.6(4) ? C28 C29 C30 C25 . . . . -1.6(6) ? C28 C29 C30 N3 . . . . -177.1(4) ? C36 C31 C32 C33 . . . . 2.0(7) ? S3 C31 C32 C33 . . . . -179.1(4) ? C31 C32 C33 C34 . . . . -1.4(8) ? C32 C33 C34 C35 . . . . -0.7(9) ? C33 C34 C35 C36 . . . . 2.2(9) ? C32 C31 C36 C35 . . . . -0.6(7) ? S3 C31 C36 C35 . . . . -179.4(4) ? C34 C35 C36 C31 . . . . -1.6(8) ? C7 C8 N1 C1 . . . . 1.3(4) ? C15 C8 N1 C1 . . . . -170.3(3) ? C7 C8 N1 S1 . . . . -138.7(3) ? C15 C8 N1 S1 . . . . 49.7(4) ? C6 C1 N1 C8 . . . . -0.5(4) ? C2 C1 N1 C8 . . . . 177.0(4) ? C6 C1 N1 S1 . . . . 140.9(3) ? C2 C1 N1 S1 . . . . -41.6(5) ? C8 C15 N2 C22 . . . . -80.9(4) ? C8 C15 N2 S2 . . . . 146.3(3) ? C23 C22 N2 C15 . . . . 55.1(4) ? C23 C22 N2 S2 . . . . -171.5(3) ? C25 C30 N3 C23 . . . . 0.3(4) ? C29 C30 N3 C23 . . . . 176.2(4) ? C25 C30 N3 S3 . . . . 146.3(3) ? C29 C30 N3 S3 . . . . -37.7(5) ? C24 C23 N3 C30 . . . . 0.2(4) ? C22 C23 N3 C30 . . . . -176.6(3) ? C24 C23 N3 S3 . . . . -145.4(3) ? C22 C23 N3 S3 . . . . 37.8(5) ? C8 N1 S1 O1 . . . . -168.6(3) ? C1 N1 S1 O1 . . . . 55.9(3) ? C8 N1 S1 O2 . . . . -39.6(3) ? C1 N1 S1 O2 . . . . -175.2(3) ? C8 N1 S1 C9 . . . . 76.1(3) ? C1 N1 S1 C9 . . . . -59.4(3) ? C14 C9 S1 O1 . . . . 163.0(3) ? C10 C9 S1 O1 . . . . -17.0(4) ? C14 C9 S1 O2 . . . . 30.0(4) ? C10 C9 S1 O2 . . . . -150.0(3) ? C14 C9 S1 N1 . . . . -84.3(3) ? C10 C9 S1 N1 . . . . 95.7(3) ? C15 N2 S2 O3 . . . . -45.1(3) ? C22 N2 S2 O3 . . . . -179.5(3) ? C15 N2 S2 O4 . . . . -174.9(3) ? C22 N2 S2 O4 . . . . 50.7(3) ? C15 N2 S2 C16 . . . . 70.8(3) ? C22 N2 S2 C16 . . . . -63.6(3) ? C21 C16 S2 O3 . . . . 39.1(4) ? C17 C16 S2 O3 . . . . -146.4(3) ? C21 C16 S2 O4 . . . . 170.9(4) ? C17 C16 S2 O4 . . . . -14.6(4) ? C21 C16 S2 N2 . . . . -75.3(4) ? C17 C16 S2 N2 . . . . 99.2(4) ? C30 N3 S3 O5 . . . . 40.2(3) ? C23 N3 S3 O5 . . . . -178.7(3) ? C30 N3 S3 O6 . . . . 169.8(3) ? C23 N3 S3 O6 . . . . -49.1(3) ? C30 N3 S3 C31 . . . . -75.2(3) ? C23 N3 S3 C31 . . . . 65.8(3) ? C36 C31 S3 O5 . . . . 134.2(3) ? C32 C31 S3 O5 . . . . -44.7(4) ? C36 C31 S3 O6 . . . . 1.1(4) ? C32 C31 S3 O6 . . . . -177.8(3) ? C36 C31 S3 N3 . . . . -112.9(3) ? C32 C31 S3 N3 . . . . 68.2(4) ?