#------------------------------------------------------------------------------ #$Date: 2021-07-03 08:04:41 +0300 (Sat, 03 Jul 2021) $ #$Revision: 266935 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/38/2243862.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_2243862 loop_ _publ_author_name 'Sribala, R.' 'Srinivasan, N.' 'Rajalaksmi, P.' 'Indumathi, S.' 'Krishnakumar, R.V.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of a pyrrolo-thiazine complex ; _journal_coeditor_code JY2008 _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 770 _journal_page_last 774 _journal_paper_doi 10.1107/S2056989021006642 _journal_volume 77 _journal_year 2021 _chemical_formula_iupac 'C22 H28 N O6 S3' _chemical_formula_moiety 'C22 H28 N O6 S3' _chemical_formula_sum 'C22 H28 N O6 S3' _chemical_formula_weight 498.66 _chemical_name_systematic 'Diethyl 2,2-dioxo-4-(thiophen-2-yl)-1-[(thiophen-2-yl)methyl]-3,4,6,7,8,8a-hexahydro-1H-pyrrolo[2,1-c][1,4]thiazine-1,3-dicarboxylate' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 76.0070(10) _cell_angle_beta 65.5840(10) _cell_angle_gamma 63.2130(10) _cell_formula_units_Z 2 _cell_length_a 10.6886(5) _cell_length_b 11.4878(5) _cell_length_c 11.8389(6) _cell_measurement_reflns_used 6274 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 60.306 _cell_measurement_theta_min 4.796 _cell_volume 1178.87(10) _computing_cell_refinement ; SAINT (Bruker, 2009) ; _computing_data_collection ; APEX2 (Bruker, 2009) ; _computing_data_reduction ; SAINT (Bruker, 2009) ; _computing_molecular_graphics ; PLUTON (Spek, 2020) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS2013/1 (Sheldrick, 2008) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_unetI/netI 0.0154 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 21855 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_min 2.280 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2009) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_meas 1.40 _exptl_crystal_density_method 'floatation method' _exptl_crystal_description needle _exptl_crystal_F_000 526 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.325 _refine_diff_density_min -0.563 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 4375 _refine_ls_number_restraints 90 _refine_ls_restrained_S_all 1.071 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0439 _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^)+(0.0758P)^2^+0.5387P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1271 _refine_ls_wR_factor_ref 0.1342 _reflns_number_gt 3774 _reflns_number_total 4375 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jy2008sup1.cif _cod_data_source_block I _cod_database_code 2243862 _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 0.901 _shelx_estimated_absorpt_t_max 0.966 _shelx_hkl_file ; -1 0 0 421.29 11.72 -1 0 0 521.84 11.86 -1 0 0 393.78 11.60 -1 0 0 494.81 12.16 1 0 0 470.61 11.64 1 0 0 512.95 11.78 1 0 0 505.74 12.20 -2 0 0 2131.64 52.08 -2 0 0 2086.98 52.58 2 0 0 2127.55 50.89 2 0 0 2179.55 50.72 2 0 0 2103.24 52.16 2 0 0 2154.77 52.01 -2 0 0 2058.90 50.96 -2 0 0 2091.35 50.99 -2 0 0 2101.36 50.87 3 0 0 0.23 0.45 3 0 0 1.00 0.44 -3 0 0 0.67 0.43 -3 0 0 0.17 0.33 3 0 0 0.65 0.46 -3 0 0 -0.08 0.37 -3 0 0 0.31 0.37 -3 0 0 0.31 0.42 4 0 0 2689.05 64.09 4 0 0 2644.60 65.83 -4 0 0 2812.66 65.94 -4 0 0 2703.65 64.23 -4 0 0 2570.09 65.81 4 0 0 2678.96 64.07 -4 0 0 2683.32 63.96 -4 0 0 2644.85 64.29 -5 0 0 83.97 2.97 5 0 0 79.44 2.96 -5 0 0 87.93 3.19 5 0 0 83.57 3.02 -5 0 0 78.84 3.00 5 0 0 84.85 2.99 -5 0 0 78.60 3.00 -5 0 0 80.50 2.82 -6 0 0 221.74 6.58 -6 0 0 200.87 6.29 -6 0 0 199.46 6.21 6 0 0 200.75 6.12 6 0 0 204.38 6.25 -6 0 0 206.80 6.17 -6 0 0 202.42 5.90 -7 0 0 3.10 0.98 7 0 0 3.28 1.05 -7 0 0 1.64 0.88 -7 0 0 2.31 1.09 -7 0 0 3.89 1.03 -7 0 0 2.78 1.05 7 0 0 2.78 0.98 8 0 0 20.51 1.88 -8 0 0 19.02 1.78 -8 0 0 23.71 1.88 -8 0 0 16.19 1.69 -8 0 0 20.40 1.89 -9 0 0 108.02 4.74 9 0 0 106.42 4.60 -9 0 0 115.97 4.82 -10 0 0 2.48 1.43 10 0 0 1.17 1.26 -10 0 0 -0.91 1.03 11 0 0 3.07 1.60 -11 0 0 4.95 1.66 -11 0 0 3.61 1.46 12 0 0 1.00 1.63 -12 0 0 1.38 1.57 13 0 0 1.71 1.81 -13 0 0 1.60 1.57 13 -1 0 9.51 2.31 12 -1 0 28.10 3.03 -12 1 0 20.99 2.80 11 -1 0 2.40 1.65 -11 1 0 -0.13 1.24 10 -1 0 12.75 2.03 -10 1 0 10.66 2.06 -10 1 0 10.34 1.93 -9 1 0 82.61 4.16 -9 1 0 78.17 4.19 9 -1 0 80.69 4.08 8 -1 0 100.70 4.39 -8 1 0 105.46 4.16 -8 1 0 99.62 4.40 -8 1 0 110.35 4.59 7 -1 0 359.58 10.58 -7 1 0 361.31 10.68 -7 1 0 367.43 10.11 7 -1 0 359.90 10.40 -7 1 0 374.59 10.52 -7 1 0 359.43 10.55 -6 1 0 31.28 2.02 -6 1 0 31.42 2.20 6 -1 0 37.73 2.17 6 -1 0 35.54 2.15 -6 1 0 33.77 2.09 -6 1 0 29.39 1.99 -6 1 0 32.38 2.15 -5 1 0 0.99 0.67 5 -1 0 0.64 0.64 5 -1 0 1.21 0.76 -5 1 0 0.92 0.70 -5 1 0 0.87 0.73 5 -1 0 0.53 0.77 -5 1 0 2.81 0.72 -5 1 0 1.48 0.62 -4 1 0 0.07 0.47 -4 1 0 1.85 0.66 -4 1 0 0.33 0.54 4 -1 0 0.31 0.56 4 -1 0 0.21 0.55 -4 1 0 -0.22 0.52 4 -1 0 0.96 0.57 -4 1 0 0.18 0.60 -3 1 0 423.62 11.16 3 -1 0 417.44 11.19 3 -1 0 424.63 10.84 -3 1 0 423.50 10.92 3 -1 0 420.01 10.82 -3 1 0 434.84 10.90 -3 1 0 418.08 10.76 -3 1 0 440.50 11.27 -2 1 0 377.33 10.08 2 -1 0 392.36 9.83 2 -1 0 386.38 9.81 2 -1 0 404.46 10.10 -2 1 0 391.50 9.79 -2 1 0 386.37 9.83 2 -1 0 382.74 10.14 -2 1 0 394.77 9.89 -2 1 0 398.17 10.17 -1 1 0 1976.50 47.19 -1 1 0 1984.40 47.12 -1 1 0 1868.79 48.54 -1 1 0 1963.82 48.32 1 -1 0 1999.91 48.29 1 -1 0 1929.07 48.71 1 -1 0 2003.18 47.45 1 -1 0 1946.05 47.12 -1 1 0 2015.23 47.61 0 1 0 1120.13 28.15 0 1 0 1153.17 28.16 0 1 0 1120.30 29.24 -2 -1 0 314.81 8.00 -2 -1 0 320.15 8.22 2 1 0 316.89 8.17 2 1 0 332.17 7.93 2 1 0 321.74 7.95 -2 -1 0 318.77 8.03 2 1 0 321.96 7.96 2 1 0 323.21 8.23 -3 -1 0 73.73 2.22 -3 -1 0 76.05 2.31 3 1 0 79.10 2.31 3 1 0 81.81 2.34 3 1 0 76.84 2.29 -3 -1 0 77.29 2.28 3 1 0 76.97 2.34 3 1 0 79.96 2.30 -3 -1 0 73.18 2.34 -4 -1 0 3.27 0.53 -4 -1 0 3.37 0.51 4 1 0 2.78 0.56 4 1 0 3.07 0.52 -4 -1 0 2.09 0.52 4 1 0 3.02 0.55 -4 -1 0 3.48 0.56 -4 -1 0 3.07 0.55 4 1 0 2.94 0.57 -5 -1 0 2.90 0.66 -5 -1 0 3.30 0.63 5 1 0 4.28 0.68 5 1 0 4.85 0.74 -5 -1 0 4.03 0.66 -5 -1 0 3.54 0.72 -5 -1 0 4.56 0.70 -6 -1 0 89.41 3.15 6 1 0 84.63 3.10 -6 -1 0 86.53 3.20 -6 -1 0 93.55 3.44 -6 -1 0 86.78 2.95 6 1 0 84.05 3.15 -6 -1 0 87.46 3.22 -7 -1 0 28.49 1.95 -7 -1 0 37.35 2.07 -7 -1 0 33.77 2.30 7 1 0 32.41 1.96 -7 -1 0 34.59 1.90 -7 -1 0 29.44 2.02 7 1 0 33.35 2.09 8 1 0 4.45 1.20 -8 -1 0 6.40 1.25 -8 -1 0 8.30 1.14 -8 -1 0 4.99 1.11 -8 -1 0 8.29 1.27 -9 -1 0 -0.10 1.03 9 1 0 1.43 1.16 -9 -1 0 -0.76 0.90 -9 -1 0 0.83 1.15 -10 -1 0 3.94 1.26 10 1 0 1.10 1.22 -10 -1 0 2.12 1.14 -11 -1 0 2.56 1.24 -11 -1 0 3.15 1.43 11 1 0 0.36 1.28 12 1 0 7.37 1.86 -12 -1 0 9.05 1.85 -12 -1 0 8.28 1.92 13 1 0 0.50 1.58 -13 -1 0 0.36 1.35 14 1 0 3.15 1.86 12 -2 0 7.56 2.25 -12 2 0 5.87 2.05 -11 2 0 -0.89 1.34 11 -2 0 -0.94 1.48 -10 2 0 -1.11 1.29 10 -2 0 0.28 1.36 -9 2 0 23.02 2.42 9 -2 0 21.46 2.24 8 -2 0 26.63 2.40 -8 2 0 24.87 2.40 -8 2 0 23.84 2.24 -8 2 0 23.21 2.13 7 -2 0 76.26 3.67 -7 2 0 76.27 3.78 -7 2 0 75.47 3.66 7 -2 0 77.65 3.73 -7 2 0 79.99 3.57 6 -2 0 6.94 1.31 -6 2 0 4.95 1.12 -6 2 0 8.00 1.26 -6 2 0 3.63 1.12 -6 2 0 8.09 1.36 6 -2 0 7.73 1.32 -5 2 0 0.39 0.80 -5 2 0 0.97 0.84 -5 2 0 0.31 0.79 5 -2 0 1.02 0.84 -5 2 0 0.61 0.67 5 -2 0 -0.40 0.66 -4 2 0 0.07 0.64 4 -2 0 0.37 0.67 -4 2 0 -0.05 0.55 4 -2 0 -0.12 0.65 4 -2 0 -0.85 0.55 -4 2 0 -0.18 0.60 -4 2 0 -0.13 0.48 3 -2 0 124.61 4.14 3 -2 0 122.94 3.96 -3 2 0 130.73 4.05 -3 2 0 126.68 3.92 -3 2 0 135.72 4.25 -3 2 0 126.63 4.09 3 -2 0 124.28 3.90 3 -2 0 125.86 3.98 -3 2 0 132.95 4.02 -2 2 0 0.14 0.36 -2 2 0 0.02 0.39 2 -2 0 -0.29 0.41 -2 2 0 0.30 0.33 2 -2 0 0.26 0.37 2 -2 0 -0.41 0.37 2 -2 0 0.01 0.18 -2 2 0 0.28 0.39 2 -2 0 -0.33 0.41 -2 2 0 -0.50 0.45 1 -2 0 409.70 10.31 1 -2 0 412.17 10.28 -1 2 0 420.01 10.66 1 -2 0 414.18 10.58 -1 2 0 417.83 10.30 1 -2 0 410.37 10.36 1 -2 0 407.95 10.66 -1 2 0 395.28 10.54 0 2 0 43.93 1.41 0 2 0 42.10 1.37 0 2 0 41.14 1.43 0 -2 0 42.78 1.37 0 2 0 42.92 1.40 0 -2 0 43.02 1.41 0 -2 0 41.91 1.46 0 -2 0 40.93 1.36 0 2 0 41.68 1.39 0 -2 0 42.38 1.40 0 2 0 44.27 1.39 1 2 0 0.04 0.18 1 2 0 0.02 0.12 -1 -2 0 -0.08 0.19 1 2 0 0.28 0.14 1 2 0 -0.06 0.15 1 2 0 -0.31 0.16 -1 -2 0 0.09 0.12 -1 -2 0 -0.06 0.04 -1 -2 0 0.10 0.12 -1 -2 0 0.01 0.05 -1 -2 0 0.24 0.16 -1 -2 0 0.28 0.15 -2 -2 0 829.30 20.87 -2 -2 0 857.01 22.24 2 2 0 853.11 22.14 2 2 0 850.23 21.92 -2 -2 0 842.36 22.43 -3 -2 0 6.53 0.43 3 2 0 7.24 0.54 3 2 0 7.80 0.44 -3 -2 0 9.11 0.78 -3 -2 0 6.54 0.52 -3 -2 0 8.73 0.52 -3 -2 0 6.60 0.47 3 2 0 6.40 0.58 3 2 0 6.65 0.40 -4 -2 0 10.41 0.81 -4 -2 0 10.96 0.75 -4 -2 0 11.18 0.65 4 2 0 10.09 0.79 -4 -2 0 10.96 0.74 -4 -2 0 10.56 0.71 4 2 0 9.27 0.68 4 2 0 12.01 0.88 -5 -2 0 76.18 2.53 5 2 0 80.06 2.59 -5 -2 0 76.99 2.62 5 2 0 78.22 2.50 -5 -2 0 73.38 2.56 5 2 0 83.90 2.61 6 2 0 480.24 12.30 -6 -2 0 469.62 12.49 -6 -2 0 475.29 12.27 6 2 0 462.84 12.11 -6 -2 0 479.97 12.20 -7 -2 0 53.21 2.44 -7 -2 0 59.82 2.72 7 2 0 54.25 2.29 -7 -2 0 55.09 2.49 -7 -2 0 54.35 2.44 7 2 0 57.93 2.51 -8 -2 0 85.15 3.44 -8 -2 0 88.21 3.58 8 2 0 86.62 3.46 -8 -2 0 83.03 3.45 -9 -2 0 1.93 1.03 9 2 0 -1.05 0.92 -9 -2 0 -0.25 0.89 -9 -2 0 0.65 0.89 10 2 0 3.15 1.23 -10 -2 0 5.50 1.32 -10 -2 0 3.53 1.28 -10 -2 0 3.41 1.17 -11 -2 0 32.57 2.72 11 2 0 26.17 2.40 -11 -2 0 27.65 2.45 -12 -2 0 3.49 1.56 12 2 0 2.55 1.48 -12 -2 0 1.23 1.28 -13 -2 0 8.56 2.00 -13 -2 0 8.76 1.95 13 2 0 11.65 2.09 14 2 0 0.53 1.73 12 -3 0 2.82 1.99 -12 3 0 0.04 1.71 11 -3 0 1.51 1.83 -11 3 0 -0.69 1.50 10 -3 0 3.40 1.80 -10 3 0 1.78 1.56 9 -3 0 0.47 1.43 -9 3 0 4.97 1.59 8 -3 0 23.22 2.32 -8 3 0 26.73 2.50 -8 3 0 28.85 2.38 -7 3 0 192.75 6.83 -7 3 0 201.79 6.50 7 -3 0 187.87 6.78 7 -3 0 179.55 6.60 -7 3 0 188.57 6.82 6 -3 0 25.35 2.21 -6 3 0 21.26 1.97 -6 3 0 20.93 1.94 6 -3 0 22.71 2.05 -6 3 0 21.78 2.03 5 -3 0 470.02 13.19 -5 3 0 473.58 12.80 5 -3 0 468.99 12.74 -5 3 0 468.37 12.59 -5 3 0 452.07 13.04 -5 3 0 474.45 12.89 4 -3 0 38.53 2.09 -4 3 0 34.06 2.10 -4 3 0 31.96 1.95 4 -3 0 35.69 1.96 4 -3 0 31.70 2.10 -4 3 0 35.82 2.02 -4 3 0 31.96 1.96 4 -3 0 33.43 2.02 3 -3 0 3.29 0.79 -3 3 0 4.33 0.80 -3 3 0 5.10 0.79 3 -3 0 7.67 0.96 -3 3 0 4.98 0.81 3 -3 0 6.04 0.93 -3 3 0 5.51 0.89 2 -3 0 261.98 7.00 -2 3 0 263.39 7.00 2 -3 0 260.14 7.33 2 -3 0 259.70 6.99 -2 3 0 226.72 6.97 2 -3 0 263.58 7.04 -2 3 0 256.58 7.20 1 -3 0 885.65 22.53 1 -3 0 890.18 21.78 -1 3 0 926.95 22.52 1 -3 0 915.20 21.95 1 -3 0 892.53 21.86 -1 3 0 825.99 21.84 -1 3 0 890.29 21.78 -1 3 0 890.40 22.41 1 -3 0 912.55 22.41 1 -3 0 881.76 21.77 0 -3 0 21.68 1.14 0 3 0 19.49 1.06 0 3 0 18.10 0.95 0 3 0 16.92 1.00 0 3 0 15.58 1.01 0 -3 0 18.27 1.01 0 -3 0 17.96 0.93 0 -3 0 16.90 0.96 0 -3 0 15.78 0.95 0 -3 0 18.39 0.99 0 -3 0 17.49 0.92 -1 -3 0 1924.36 46.66 -1 -3 0 1885.93 46.19 1 3 0 1929.02 46.85 -1 -3 0 1966.86 46.56 1 3 0 1940.28 46.24 -1 -3 0 1902.68 46.28 -1 -3 0 1913.36 47.71 1 3 0 1895.94 47.32 1 3 0 1968.36 45.89 1 3 0 1935.77 47.67 -1 -3 0 1872.32 46.14 -2 -3 0 10.88 0.55 2 3 0 11.15 0.44 2 3 0 10.76 0.44 -2 -3 0 9.73 0.78 2 3 0 11.28 0.60 2 3 0 10.79 0.61 -2 -3 0 14.04 0.59 2 3 0 11.16 0.59 -2 -3 0 11.49 0.50 -3 -3 0 39.89 1.73 -3 -3 0 41.16 1.28 -3 -3 0 42.65 1.30 -3 -3 0 41.71 1.22 3 3 0 42.37 1.23 -3 -3 0 40.22 1.20 3 3 0 43.76 1.25 -4 -3 0 5233.30 127.94 4 3 0 5331.57 124.31 4 3 0 5189.93 124.96 -4 -3 0 5244.05 128.61 -4 -3 0 4954.00 124.61 -4 -3 0 5214.28 125.78 -4 -3 0 5118.70 125.64 -5 -3 0 288.24 7.54 5 3 0 296.23 7.48 -5 -3 0 298.82 7.78 5 3 0 303.07 7.48 -5 -3 0 286.97 7.70 -5 -3 0 288.96 7.50 5 3 0 284.52 7.48 6 3 0 156.93 4.32 -6 -3 0 146.61 4.41 -6 -3 0 143.97 4.28 6 3 0 150.28 4.12 6 3 0 145.65 4.31 -6 -3 0 151.77 4.53 -6 -3 0 144.68 4.36 -7 -3 0 50.18 2.13 -7 -3 0 49.30 2.17 7 3 0 50.86 2.15 -7 -3 0 50.28 2.25 7 3 0 45.77 1.85 -7 -3 0 41.82 2.18 -8 -3 0 313.76 8.55 -8 -3 0 302.77 8.69 -8 -3 0 298.32 8.59 8 3 0 295.64 8.39 -9 -3 0 0.15 0.82 -9 -3 0 1.16 1.02 -9 -3 0 0.21 0.86 9 3 0 1.24 1.01 -10 -3 0 56.73 3.11 -10 -3 0 68.33 3.22 10 3 0 60.57 3.06 -10 -3 0 56.03 3.01 11 3 0 9.61 1.57 -11 -3 0 6.63 1.50 -11 -3 0 7.88 1.45 -12 -3 0 1.13 1.22 -12 -3 0 0.54 1.25 12 3 0 0.54 1.29 -13 -3 0 11.45 2.01 13 3 0 14.90 2.11 -13 -3 0 15.54 2.18 -14 -3 0 -0.08 1.61 14 3 0 -0.34 1.43 -11 4 0 -2.68 1.60 11 -4 0 -0.27 1.68 -10 4 0 -0.32 1.53 10 -4 0 -1.36 1.45 9 -4 0 2.44 1.53 -9 4 0 0.35 1.35 -8 4 0 11.94 1.94 -8 4 0 12.37 1.97 8 -4 0 12.35 1.98 7 -4 0 0.30 1.06 -7 4 0 0.11 1.24 -7 4 0 1.25 1.23 7 -4 0 -1.18 1.19 6 -4 0 59.18 3.42 6 -4 0 57.80 3.33 -6 4 0 54.40 3.18 -6 4 0 62.76 3.48 -6 4 0 59.32 3.14 -5 4 0 57.28 3.05 -5 4 0 57.16 3.04 5 -4 0 50.58 2.97 -5 4 0 52.21 2.94 5 -4 0 51.87 3.02 4 -4 0 118.01 4.52 -4 4 0 119.23 4.30 -4 4 0 122.50 4.45 -4 4 0 107.69 4.28 4 -4 0 110.58 4.30 3 -4 0 0.28 0.65 3 -4 0 -0.79 0.73 -3 4 0 0.61 0.67 3 -4 0 0.89 0.59 -3 4 0 -0.41 0.70 -3 4 0 0.97 0.66 3 -4 0 -0.04 0.73 2 -4 0 13.42 1.18 -2 4 0 13.69 1.19 2 -4 0 11.50 1.06 -2 4 0 13.64 1.20 2 -4 0 10.90 1.12 2 -4 0 10.74 1.09 2 -4 0 10.20 1.12 1 -4 0 6.65 0.80 1 -4 0 4.85 0.75 1 -4 0 7.39 0.81 1 -4 0 5.80 0.76 1 -4 0 7.97 0.85 -1 4 0 4.50 0.69 -1 4 0 6.37 0.81 1 -4 0 4.95 0.76 0 -4 0 27.16 1.31 0 -4 0 28.57 1.28 0 -4 0 27.74 1.37 0 -4 0 27.08 1.44 0 -4 0 26.74 1.29 0 4 0 29.23 1.38 0 -4 0 25.31 1.29 0 -4 0 28.44 1.40 0 4 0 27.70 1.44 1 4 0 14.95 0.98 -1 -4 0 14.33 0.95 1 4 0 14.70 0.86 1 4 0 15.09 1.03 1 4 0 14.66 0.96 -1 -4 0 15.33 0.90 -1 -4 0 14.97 0.96 -1 -4 0 14.34 0.86 -1 -4 0 14.05 0.85 -1 -4 0 14.35 0.86 -1 -4 0 14.81 0.90 -2 -4 0 8.80 0.64 2 4 0 8.46 0.56 -2 -4 0 7.88 0.52 -2 -4 0 8.77 0.61 -2 -4 0 6.56 0.72 2 4 0 8.44 0.62 2 4 0 10.48 0.72 2 4 0 9.18 0.73 -2 -4 0 9.18 0.67 -2 -4 0 9.14 0.67 2 4 0 9.25 0.58 -2 -4 0 7.00 0.59 -3 -4 0 26.98 0.93 -3 -4 0 25.31 1.00 -3 -4 0 28.80 1.04 -3 -4 0 24.60 1.43 3 4 0 28.15 0.99 3 4 0 28.60 1.01 4 4 0 2251.26 54.40 -4 -4 0 2237.23 55.40 4 4 0 2300.91 54.34 -4 -4 0 2317.41 55.82 -4 -4 0 2221.63 55.06 -4 -4 0 2281.11 55.43 -4 -4 0 2214.08 56.09 -5 -4 0 869.40 21.22 -5 -4 0 863.72 21.71 -5 -4 0 858.10 21.16 5 4 0 899.69 21.03 -5 -4 0 878.26 21.69 5 4 0 856.50 21.07 -5 -4 0 861.31 22.10 -6 -4 0 67.14 2.30 -6 -4 0 68.38 2.39 6 4 0 66.44 2.25 -6 -4 0 64.03 2.29 -6 -4 0 64.01 2.21 6 4 0 68.48 2.29 -7 -4 0 24.35 1.59 7 4 0 22.14 1.46 -7 -4 0 21.64 1.40 -7 -4 0 22.82 1.43 -7 -4 0 24.58 1.39 7 4 0 24.21 1.48 -8 -4 0 133.14 4.32 8 4 0 131.53 4.27 -8 -4 0 130.19 4.37 -8 -4 0 144.01 4.62 -8 -4 0 132.02 4.45 -9 -4 0 159.96 5.17 -9 -4 0 156.91 5.27 9 4 0 153.77 5.08 -9 -4 0 159.61 5.25 -10 -4 0 45.76 2.56 -10 -4 0 47.06 2.65 -10 -4 0 47.78 2.62 10 4 0 45.39 2.55 -11 -4 0 3.45 1.17 11 4 0 2.94 1.12 -11 -4 0 3.24 1.25 -11 -4 0 4.82 1.24 -12 -4 0 5.70 1.40 -12 -4 0 4.72 1.51 12 4 0 6.89 1.44 -13 -4 0 9.06 1.76 13 4 0 9.67 1.83 -13 -4 0 6.53 1.79 -14 -4 0 -0.90 1.32 -14 -4 0 1.69 1.60 14 4 0 2.22 1.54 -11 5 0 -0.60 1.74 11 -5 0 1.92 1.88 10 -5 0 4.41 2.11 -10 5 0 6.16 2.20 -9 5 0 4.14 1.87 9 -5 0 2.65 1.70 8 -5 0 20.04 2.54 -8 5 0 15.88 2.29 -8 5 0 18.80 2.30 7 -5 0 6.13 1.71 -7 5 0 3.03 1.41 7 -5 0 5.21 1.50 -7 5 0 4.39 1.59 -6 5 0 12.75 1.79 6 -5 0 14.55 1.90 -6 5 0 12.98 1.89 6 -5 0 9.75 1.69 -5 5 0 187.44 6.40 5 -5 0 175.60 6.35 5 -5 0 190.28 6.82 -5 5 0 186.03 6.58 -4 5 0 1111.25 28.74 4 -5 0 1140.22 29.90 -4 5 0 1146.98 29.71 -4 5 0 1171.42 29.13 4 -5 0 1150.15 28.91 3 -5 0 736.63 19.82 3 -5 0 755.77 19.20 -3 5 0 724.16 19.59 3 -5 0 751.72 19.12 -3 5 0 733.47 19.04 -2 5 0 15.98 1.46 -2 5 0 14.56 1.30 2 -5 0 17.31 1.47 2 -5 0 13.15 1.33 2 -5 0 14.49 1.32 -2 5 0 12.90 1.24 2 -5 0 14.13 1.37 2 -5 0 12.82 1.35 1 -5 0 249.07 6.97 1 -5 0 252.59 7.10 -1 5 0 234.12 7.02 1 -5 0 232.27 7.21 1 -5 0 241.56 6.85 1 -5 0 242.05 6.85 -1 5 0 244.00 6.92 1 -5 0 257.92 7.18 0 -5 0 538.13 13.65 0 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6.96 -7 -5 0 82.44 2.79 7 5 0 79.88 2.72 -7 -5 0 90.60 2.94 -7 -5 0 81.88 2.71 7 5 0 81.87 2.72 -7 -5 0 81.09 2.76 -8 -5 0 42.59 2.08 -8 -5 0 39.66 1.90 -8 -5 0 35.32 1.84 -8 -5 0 39.37 1.97 8 5 0 39.98 1.90 -9 -5 0 9.00 1.22 -9 -5 0 10.07 1.20 9 5 0 9.95 1.18 -9 -5 0 10.22 1.15 -10 -5 0 184.40 5.89 -10 -5 0 188.60 6.04 10 5 0 184.90 5.79 -10 -5 0 177.83 5.91 -11 -5 0 -0.14 0.92 11 5 0 0.97 0.95 -11 -5 0 1.16 0.91 -11 -5 0 0.02 0.86 -12 -5 0 17.15 1.79 -12 -5 0 14.47 1.75 12 5 0 15.98 1.75 -12 -5 0 14.81 1.91 -13 -5 0 -0.17 1.23 13 5 0 0.62 1.24 -13 -5 0 -2.08 0.94 14 5 0 -1.18 1.24 -14 -5 0 0.31 1.30 -14 -5 0 1.81 1.53 -10 6 0 -1.61 1.76 10 -6 0 -0.13 1.75 9 -6 0 -0.77 1.66 -9 6 0 1.85 1.75 -8 6 0 1.51 1.59 8 -6 0 4.47 1.86 -8 6 0 3.77 1.65 -7 6 0 8.73 1.95 7 -6 0 4.73 1.70 -7 6 0 9.36 1.98 -6 6 0 0.54 1.25 6 -6 0 3.30 1.43 6 -6 0 1.77 1.38 -6 6 0 1.54 1.38 5 -6 0 9.74 1.73 -5 6 0 12.68 1.81 -5 6 0 12.76 1.82 5 -6 0 12.73 1.82 -4 6 0 18.58 1.92 4 -6 0 14.00 1.80 -4 6 0 16.49 1.87 4 -6 0 14.29 1.86 -3 6 0 1213.63 31.33 3 -6 0 1232.03 30.52 3 -6 0 1190.15 31.56 3 -6 0 1250.68 30.64 -3 6 0 1179.58 30.40 2 -6 0 4.11 0.95 2 -6 0 1.64 1.00 -2 6 0 2.47 1.10 2 -6 0 3.96 1.03 2 -6 0 5.36 1.02 -2 6 0 3.90 0.99 1 -6 0 16.80 1.38 1 -6 0 15.88 1.42 1 -6 0 16.26 1.43 1 -6 0 16.87 1.21 -1 6 0 12.85 1.32 -1 6 0 16.05 1.39 1 -6 0 15.56 1.48 0 6 0 784.45 20.48 0 -6 0 805.61 20.24 0 -6 0 784.99 20.79 0 -6 0 856.62 20.73 0 6 0 778.50 19.99 0 -6 0 784.89 19.91 0 -6 0 792.59 20.11 0 -6 0 801.48 20.01 1 6 0 606.28 15.52 -1 -6 0 634.43 15.78 -1 -6 0 629.43 15.78 -1 -6 0 601.86 15.64 1 6 0 614.81 15.59 1 6 0 618.79 15.92 -1 -6 0 611.28 15.46 -1 -6 0 605.17 16.18 -1 -6 0 649.28 16.13 -2 -6 0 318.68 8.81 -2 -6 0 329.73 8.56 -2 -6 0 341.81 8.88 2 6 0 325.90 8.55 2 6 0 327.78 8.46 -2 -6 0 288.18 8.19 2 6 0 332.44 8.45 -2 -6 0 331.39 8.53 3 6 0 1110.18 26.07 -3 -6 0 1049.87 26.89 3 6 0 1089.27 26.00 -3 -6 0 1080.97 26.23 -3 -6 0 1105.61 26.87 3 6 0 1053.55 26.07 -3 -6 0 1062.24 26.19 -3 -6 0 1047.74 26.91 3 6 0 1090.49 26.65 4 6 0 2.54 0.49 4 6 0 4.29 0.52 -4 -6 0 1.79 0.41 -4 -6 0 2.21 0.48 4 6 0 3.49 0.53 -4 -6 0 2.52 0.47 -4 -6 0 1.58 0.69 -5 -6 0 450.75 11.32 -5 -6 0 451.46 12.41 -5 -6 0 447.23 11.61 5 6 0 461.39 11.23 5 6 0 456.07 11.25 -5 -6 0 463.74 11.61 6 6 0 12.49 0.95 -6 -6 0 10.31 1.31 6 6 0 10.61 0.84 -6 -6 0 10.44 0.80 -6 -6 0 10.70 0.74 -6 -6 0 12.39 0.90 -6 -6 0 11.18 0.82 -7 -6 0 47.10 1.83 7 6 0 52.02 1.93 -7 -6 0 53.06 1.93 -7 -6 0 54.61 2.05 7 6 0 50.36 1.94 -7 -6 0 49.10 1.90 -8 -6 0 2.20 0.72 -8 -6 0 2.47 0.70 -8 -6 0 2.51 0.64 8 6 0 3.48 0.76 -8 -6 0 1.92 0.62 -9 -6 0 80.89 3.00 9 6 0 77.17 2.91 -9 -6 0 78.77 3.03 -9 -6 0 79.90 2.98 -10 -6 0 -0.54 0.91 -10 -6 0 0.09 0.83 -10 -6 0 -1.11 0.72 10 6 0 -0.97 0.80 -11 -6 0 2.10 1.01 11 6 0 1.05 0.93 -11 -6 0 0.70 0.84 -11 -6 0 0.38 0.84 -12 -6 0 6.02 1.31 -12 -6 0 7.87 1.43 12 6 0 8.20 1.37 -12 -6 0 7.02 1.39 -13 -6 0 0.97 1.20 -13 -6 0 -2.21 0.93 13 6 0 -0.97 1.08 14 6 0 1.11 1.28 -14 -6 0 -0.58 1.22 -14 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2 7 0 94.62 3.25 -2 -7 0 95.42 3.26 -2 -7 0 97.87 3.04 -2 -7 0 93.92 3.46 2 7 0 95.77 3.17 2 7 0 97.64 3.26 -2 -7 0 95.13 3.45 -2 -7 0 97.85 3.39 -2 -7 0 101.08 3.40 -3 -7 0 605.50 14.66 3 7 0 605.13 15.18 -3 -7 0 597.03 15.17 -3 -7 0 600.49 15.71 -3 -7 0 595.69 15.13 3 7 0 597.04 14.98 3 7 0 587.45 15.01 -3 -7 0 592.64 15.60 3 7 0 625.64 15.08 -3 -7 0 605.44 15.52 -4 -7 0 80.20 3.29 4 7 0 82.47 2.65 -4 -7 0 78.35 2.63 4 7 0 81.66 2.63 -4 -7 0 86.84 2.78 -4 -7 0 78.17 2.75 -4 -7 0 76.57 2.60 4 7 0 80.83 2.61 -4 -7 0 80.07 2.76 5 7 0 78.62 2.50 -5 -7 0 75.35 2.57 -5 -7 0 84.42 3.47 5 7 0 78.57 2.46 -5 -7 0 82.82 2.62 -5 -7 0 75.24 2.47 5 7 0 81.08 2.53 6 7 0 24.29 1.24 -6 -7 0 23.13 1.15 6 7 0 24.86 1.24 -6 -7 0 24.04 1.25 6 7 0 23.48 1.16 -6 -7 0 23.32 1.19 -6 -7 0 22.76 1.92 -7 -7 0 19.54 1.16 -7 -7 0 16.56 1.20 7 7 0 19.79 1.19 7 7 0 19.28 1.23 -7 -7 0 19.78 1.19 -8 -7 0 26.86 1.40 -8 -7 0 27.59 1.42 -8 -7 0 27.41 1.50 -8 -7 0 28.44 1.59 8 7 0 27.88 1.47 9 7 0 13.21 1.13 -9 -7 0 13.73 1.19 -9 -7 0 12.93 1.15 -9 -7 0 13.98 1.23 -9 -7 0 13.29 1.16 -10 -7 0 1.44 0.89 -10 -7 0 3.13 0.85 -10 -7 0 1.39 0.81 10 7 0 3.46 0.92 -11 -7 0 8.21 1.15 -11 -7 0 7.01 1.25 11 7 0 8.22 1.20 -11 -7 0 10.74 1.25 -12 -7 0 48.42 2.73 12 7 0 46.20 2.63 -12 -7 0 41.62 2.70 -12 -7 0 49.52 2.64 -13 -7 0 2.11 1.11 -13 -7 0 1.67 1.14 -13 -7 0 1.38 1.22 13 7 0 1.20 1.17 -14 -7 0 0.64 1.20 -14 -7 0 1.23 1.28 14 7 0 0.57 1.25 9 -8 0 18.79 3.09 -8 8 0 2.96 1.91 8 -8 0 1.05 1.83 -7 8 0 -0.07 1.54 7 -8 0 -4.15 1.36 -7 8 0 -0.51 1.59 6 -8 0 7.76 1.98 -6 8 0 5.30 1.89 -6 8 0 8.49 2.12 6 -8 0 2.34 1.62 5 -8 0 28.90 2.79 -5 8 0 27.38 2.75 5 -8 0 27.34 2.67 -5 8 0 30.45 2.80 4 -8 0 58.16 3.75 -4 8 0 55.03 3.52 4 -8 0 56.94 3.40 -4 8 0 48.06 3.25 3 -8 0 -1.10 1.12 -3 8 0 0.24 1.11 -3 8 0 -1.03 1.17 3 -8 0 0.68 1.18 2 -8 0 52.81 2.47 2 -8 0 52.31 3.01 2 -8 0 47.90 3.12 2 -8 0 46.46 2.97 -2 8 0 51.10 3.05 -2 8 0 55.55 3.14 -1 8 0 233.30 7.32 1 -8 0 229.01 6.75 1 -8 0 232.56 7.18 1 -8 0 236.55 7.40 1 -8 0 215.19 7.58 -1 8 0 236.08 7.41 0 -8 0 309.73 8.70 0 8 0 298.25 8.85 0 -8 0 300.96 8.53 0 -8 0 313.93 8.99 0 8 0 299.47 8.92 0 -8 0 295.80 9.29 0 -8 0 333.05 9.23 -1 -8 0 201.26 6.13 1 8 0 208.75 6.25 -1 -8 0 220.37 6.58 -1 -8 0 202.46 6.03 -1 -8 0 202.61 6.28 1 8 0 194.09 6.17 -1 -8 0 203.04 6.64 -1 -8 0 205.22 6.41 2 8 0 55.55 2.57 2 8 0 57.29 2.63 -2 -8 0 58.64 2.71 -2 -8 0 59.26 2.62 -2 -8 0 59.94 2.66 -2 -8 0 56.02 2.50 2 8 0 56.94 2.36 -2 -8 0 58.66 2.67 -2 -8 0 56.47 2.28 -3 -8 0 499.63 12.79 3 8 0 492.10 12.60 -3 -8 0 485.99 13.16 -3 -8 0 476.16 13.10 3 8 0 482.93 12.59 -3 -8 0 493.60 12.14 3 8 0 485.41 12.54 -3 -8 0 494.06 12.73 4 8 0 119.04 3.64 -4 -8 0 112.51 3.77 -4 -8 0 111.27 3.62 -4 -8 0 109.69 3.61 -4 -8 0 119.25 3.77 4 8 0 113.83 3.59 -4 -8 0 109.15 4.17 4 8 0 109.37 3.57 -5 -8 0 203.08 6.63 5 8 0 202.96 5.58 -5 -8 0 198.17 5.67 5 8 0 209.19 5.63 -5 -8 0 201.39 5.85 5 8 0 211.08 5.60 -5 -8 0 202.21 5.66 -5 -8 0 198.39 5.84 -5 -8 0 211.79 5.85 -6 -8 0 0.25 0.56 -6 -8 0 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4.70 3 4 -3 184.04 4.66 -3 -4 3 184.34 5.83 -3 -4 3 190.75 4.86 -3 -4 3 179.76 4.87 -2 -4 3 38.57 2.01 -2 -4 3 37.23 1.37 2 4 -3 38.15 1.31 -2 -4 3 38.72 1.34 2 4 -3 36.10 1.30 -2 -4 3 35.97 1.26 1 4 -3 9.17 0.64 -1 -4 3 10.17 0.81 -1 -4 3 9.43 0.79 -1 -4 3 10.02 0.86 -1 -4 3 9.13 0.76 1 4 -3 11.65 0.93 -1 -4 3 9.69 0.56 1 4 -3 9.85 0.75 -1 -4 3 10.55 1.06 0 4 -3 573.84 14.12 0 -4 3 575.91 14.80 0 -4 3 586.23 14.23 0 -4 3 478.06 14.42 0 -4 3 571.92 14.65 0 -4 3 583.88 13.99 0 4 -3 573.88 14.43 0 -4 3 583.29 14.27 -1 4 -3 492.89 12.99 1 -4 3 522.36 13.15 -1 4 -3 496.59 12.70 1 -4 3 491.93 12.83 1 -4 3 481.96 13.16 1 -4 3 493.41 12.59 1 -4 3 503.04 12.81 2 -4 3 149.59 4.67 -2 4 -3 144.14 4.54 2 -4 3 139.86 4.71 2 -4 3 142.96 4.53 2 -4 3 145.06 4.63 2 -4 3 134.83 4.36 -2 4 -3 135.79 4.49 3 -4 3 60.79 2.67 3 -4 3 61.71 2.82 -3 4 -3 60.23 2.67 -3 4 -3 61.26 2.66 3 -4 3 56.83 2.58 3 -4 3 58.59 2.79 4 -4 3 10.33 1.31 4 -4 3 9.94 1.34 4 -4 3 9.83 1.36 -4 4 -3 12.28 1.43 -4 4 -3 13.78 1.46 -4 4 -3 8.38 1.31 4 -4 3 9.09 1.26 5 -4 3 97.68 4.08 5 -4 3 107.13 4.21 -5 4 -3 102.75 4.22 5 -4 3 100.59 4.31 -5 4 -3 96.98 4.19 -6 4 -3 20.86 2.06 -6 4 -3 23.66 2.18 6 -4 3 30.30 2.51 6 -4 3 20.83 2.16 7 -4 3 -1.16 1.20 -7 4 -3 1.06 1.24 -7 4 -3 -0.10 1.03 7 -4 3 -1.50 0.97 -8 4 -3 33.02 2.72 8 -4 3 33.32 2.81 -8 4 -3 36.11 2.89 8 -4 3 39.20 3.13 -9 4 -3 0.87 1.29 -9 4 -3 2.86 1.59 9 -4 3 1.08 1.60 -10 4 -3 1.80 1.53 10 -4 3 3.85 1.74 -11 4 -3 6.90 2.17 11 -4 3 3.20 2.07 12 -4 3 4.81 2.24 -12 4 -3 4.71 2.09 13 3 -3 0.53 1.52 -13 -3 3 2.96 1.62 -12 -3 3 6.61 1.74 -12 -3 3 12.23 1.89 12 3 -3 11.35 1.88 -11 -3 3 -1.23 1.10 -11 -3 3 1.16 1.16 11 3 -3 0.82 1.28 10 3 -3 10.37 1.53 -10 -3 3 7.01 1.36 -10 -3 3 8.34 1.51 -10 -3 3 7.54 1.39 -9 -3 3 29.99 2.19 -9 -3 3 33.74 2.16 -9 -3 3 30.20 2.15 9 3 -3 31.79 2.14 8 3 -3 31.06 1.97 8 3 -3 31.80 1.96 -8 -3 3 28.19 1.91 -8 -3 3 30.72 1.93 -8 -3 3 29.15 1.97 -7 -3 3 109.02 3.80 -7 -3 3 102.13 3.59 -7 -3 3 96.55 3.58 -7 -3 3 102.34 3.54 7 3 -3 99.68 3.47 -6 -3 3 68.90 2.59 -6 -3 3 67.69 3.37 -6 -3 3 70.65 2.57 6 3 -3 73.41 2.62 -6 -3 3 77.62 2.78 -6 -3 3 72.54 2.64 6 3 -3 67.62 2.55 5 3 -3 36.69 1.61 -5 -3 3 36.38 1.58 -5 -3 3 38.52 1.62 5 3 -3 42.70 1.69 5 3 -3 40.52 1.63 -5 -3 3 40.14 1.58 -5 -3 3 41.78 1.73 -5 -3 3 35.75 2.37 4 3 -3 40.86 1.43 4 3 -3 39.12 1.39 4 3 -3 41.13 1.45 -4 -3 3 40.55 2.32 -4 -3 3 41.07 1.47 -4 -3 3 40.55 1.37 -4 -3 3 41.36 1.52 -4 -3 3 40.08 1.40 -3 -3 3 129.18 3.53 3 3 -3 133.78 3.49 3 3 -3 137.08 3.52 -3 -3 3 130.17 4.45 -3 -3 3 137.40 3.56 -3 -3 3 131.00 3.64 -3 -3 3 143.07 3.69 3 3 -3 135.87 3.50 2 3 -3 8.63 0.58 -2 -3 3 8.50 0.96 -2 -3 3 8.49 0.61 -2 -3 3 8.37 0.52 -2 -3 3 9.17 0.57 2 3 -3 8.55 0.61 -1 -3 3 2023.49 48.74 -1 -3 3 1942.69 48.87 -1 -3 3 1951.68 48.43 -1 -3 3 1960.08 47.68 1 3 -3 2047.84 47.35 1 3 -3 1972.16 47.46 1 3 -3 1979.76 49.10 0 -3 3 137.98 4.36 0 3 -3 137.49 3.91 0 3 -3 138.02 3.87 0 3 -3 142.52 3.91 0 -3 3 137.32 3.94 0 -3 3 140.79 3.78 0 -3 3 137.41 4.06 0 -3 3 134.67 3.89 1 -3 3 1812.30 44.40 1 -3 3 1863.39 44.47 1 -3 3 1865.08 44.22 1 -3 3 1914.61 45.52 -1 3 -3 1805.51 45.42 1 -3 3 1809.35 45.60 -1 3 -3 1817.17 44.25 2 -3 3 1256.72 30.74 -2 3 -3 1228.92 31.41 2 -3 3 1291.62 30.84 2 -3 3 1263.75 30.58 -2 3 -3 1228.20 30.57 2 -3 3 1229.45 31.58 2 -3 3 1284.39 31.51 3 -3 3 1499.06 35.71 3 -3 3 1431.42 36.56 3 -3 3 1453.60 35.41 3 -3 3 1475.81 35.58 -3 3 -3 1424.51 35.39 -3 3 -3 1421.27 36.35 4 -3 3 29.47 1.84 4 -3 3 30.56 1.98 4 -3 3 28.34 1.96 -4 3 -3 28.46 1.84 -4 3 -3 31.23 1.96 -5 3 -3 92.50 3.71 5 -3 3 92.28 3.69 -5 3 -3 90.99 3.80 5 -3 3 91.36 3.69 -5 3 -3 90.61 3.72 5 -3 3 93.03 3.90 -6 3 -3 110.27 4.45 6 -3 3 115.19 4.42 -6 3 -3 105.43 4.40 -6 3 -3 107.44 4.31 6 -3 3 105.21 4.50 -7 3 -3 51.32 2.99 7 -3 3 46.65 3.03 -7 3 -3 49.47 3.02 7 -3 3 52.83 3.05 -8 3 -3 75.31 3.91 8 -3 3 71.53 3.88 -8 3 -3 67.43 3.59 8 -3 3 76.69 4.00 -9 3 -3 0.81 1.24 9 -3 3 1.32 1.38 -9 3 -3 1.29 1.31 10 -3 3 15.49 2.27 -10 3 -3 12.22 2.06 -11 3 -3 2.71 1.83 11 -3 3 2.96 1.93 -12 3 -3 4.26 1.97 12 -3 3 5.70 2.22 -13 -2 3 0.22 1.57 13 2 -3 2.73 1.76 12 2 -3 0.55 1.46 -12 -2 3 2.37 1.48 -12 -2 3 0.41 1.48 -11 -2 3 5.48 1.54 -11 -2 3 5.44 1.59 11 2 -3 5.03 1.51 -10 -2 3 63.35 3.50 -10 -2 3 62.70 3.41 10 2 -3 61.26 3.39 -9 -2 3 -0.45 0.89 9 2 -3 1.76 1.06 -9 -2 3 0.22 0.99 -9 -2 3 -1.11 0.87 9 2 -3 -0.86 0.93 -8 -2 3 74.93 3.30 8 2 -3 79.01 3.28 8 2 -3 72.82 3.23 -8 -2 3 75.33 3.34 -8 -2 3 75.74 3.26 -7 -2 3 82.00 3.38 7 2 -3 86.72 3.32 -7 -2 3 82.60 3.35 -7 -2 3 86.75 3.34 -6 -2 3 773.85 19.34 6 2 -3 749.36 19.21 -6 -2 3 763.25 19.83 -6 -2 3 752.52 19.39 -6 -2 3 812.66 19.99 5 2 -3 659.83 15.73 5 2 -3 622.26 15.73 -5 -2 3 613.41 16.20 -5 -2 3 652.35 16.33 -5 -2 3 624.03 15.81 -5 -2 3 621.55 15.86 -5 -2 3 628.30 16.66 -4 -2 3 229.95 6.93 -4 -2 3 228.36 6.36 4 2 -3 236.06 6.13 -4 -2 3 244.46 6.46 -4 -2 3 229.79 6.18 4 2 -3 238.30 6.17 -4 -2 3 234.81 6.23 -3 -2 3 25.47 1.10 3 2 -3 27.69 1.15 3 2 -3 29.32 1.19 3 2 -3 28.62 1.15 -3 -2 3 32.20 1.24 -3 -2 3 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127.52 5.33 10 1 4 123.09 5.06 -10 -1 -4 133.31 4.91 11 1 4 1.04 1.42 -11 -1 -4 1.49 1.26 12 1 4 2.65 1.69 -12 -1 -4 0.64 1.36 -13 -1 -4 3.86 1.65 13 1 4 1.36 1.60 -14 -1 -4 0.69 1.57 14 1 4 1.16 1.84 11 -2 -4 7.70 2.33 10 -2 -4 4.83 1.97 -10 2 4 5.88 1.95 9 -2 -4 -1.18 1.34 -9 2 4 0.60 1.40 9 -2 -4 0.15 1.45 8 -2 -4 12.10 1.84 -8 2 4 18.06 2.13 -8 2 4 13.42 1.91 8 -2 -4 12.89 1.85 -7 2 4 22.49 2.23 7 -2 -4 19.85 2.01 -7 2 4 26.01 2.25 -6 2 4 42.13 2.73 6 -2 -4 41.01 2.69 -6 2 4 41.59 2.75 -5 2 4 26.13 2.01 5 -2 -4 23.69 1.99 5 -2 -4 19.80 1.85 -5 2 4 25.53 2.03 -5 2 4 24.17 2.06 -5 2 4 24.94 2.04 4 -2 -4 68.54 3.13 -4 2 4 81.83 3.39 -4 2 4 70.24 2.91 -4 2 4 74.58 3.14 -4 2 4 73.51 3.20 -4 2 4 69.28 3.08 4 -2 -4 70.54 3.14 -3 2 4 13.47 1.26 3 -2 -4 12.38 1.28 3 -2 -4 12.20 1.19 -3 2 4 14.23 1.34 -3 2 4 11.54 1.19 -3 2 4 12.25 1.24 -3 2 4 11.85 1.25 -3 2 4 13.85 1.32 -2 2 4 986.50 24.58 -2 2 4 946.52 23.60 -2 2 4 967.84 23.87 -2 2 4 943.42 23.90 -2 2 4 929.97 24.41 2 -2 -4 946.05 24.45 2 -2 -4 944.28 23.73 -2 2 4 968.48 23.56 -2 2 4 964.11 23.60 -2 2 4 991.12 24.60 -1 2 4 2017.37 47.90 -1 2 4 2048.99 49.16 -1 2 4 1939.44 49.07 -1 2 4 2004.80 47.64 1 -2 -4 1955.62 49.09 -1 2 4 1967.08 47.93 -1 2 4 1986.13 47.95 -1 2 4 1974.19 47.46 1 -2 -4 1934.76 47.69 0 2 4 477.05 12.20 0 2 4 461.81 11.86 0 2 4 473.91 11.60 0 2 4 463.37 11.68 0 -2 -4 452.05 11.74 0 2 4 476.63 11.72 0 2 4 447.41 12.11 0 2 4 462.00 11.83 0 -2 -4 458.00 12.14 0 -2 -4 451.15 12.15 -1 -2 -4 24.67 1.31 1 2 4 24.65 1.32 1 2 4 25.44 1.37 -1 -2 -4 22.44 1.37 1 2 4 26.01 1.30 1 2 4 25.19 1.38 -1 -2 -4 21.47 1.22 1 2 4 25.39 1.33 2 2 4 48.56 1.95 2 2 4 50.00 1.91 2 2 4 49.33 1.89 -2 -2 -4 52.75 2.01 -2 -2 -4 48.44 1.90 2 2 4 49.20 1.93 -2 -2 -4 50.02 1.96 -3 -2 -4 1611.57 38.41 -3 -2 -4 1525.92 38.36 3 2 4 1521.41 37.25 -3 -2 -4 1530.52 37.45 3 2 4 1570.39 38.32 -3 -2 -4 1541.60 37.29 3 2 4 1518.37 38.37 -4 -2 -4 1045.43 25.80 4 2 4 1048.14 26.39 -4 -2 -4 1081.11 26.45 -4 -2 -4 1036.31 26.39 -4 -2 -4 1052.09 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10 6 16 2.25 2.07 11 6 16 7.91 2.43 -11 -6 -16 7.45 2.48 11 6 16 6.38 2.26 12 6 16 10.60 2.71 12 6 16 7.04 2.34 2 7 16 1.32 1.86 -2 -7 -16 2.74 2.32 -3 -7 -16 2.75 2.05 3 7 16 6.09 2.31 4 7 16 1.33 1.87 -4 -7 -16 1.07 1.97 5 7 16 -1.91 1.84 5 7 16 3.22 2.12 -5 -7 -16 -0.55 1.99 6 7 16 5.95 2.16 6 7 16 3.93 2.18 -6 -7 -16 2.60 2.16 -7 -7 -16 -0.29 1.93 7 7 16 1.07 2.08 7 7 16 1.80 1.82 -8 -7 -16 6.57 2.25 8 7 16 8.69 2.46 8 7 16 5.25 2.14 9 7 16 4.75 2.22 -9 -7 -16 1.43 1.92 9 7 16 1.43 1.98 -10 -7 -16 4.94 2.33 10 7 16 11.22 2.47 10 7 16 6.71 2.30 11 7 16 2.00 1.99 11 7 16 0.61 1.76 -11 -7 -16 -0.32 1.97 12 7 16 3.22 2.15 12 7 16 0.33 1.88 -2 -8 -16 3.07 2.29 3 8 16 3.29 1.90 -3 -8 -16 4.52 2.34 4 8 16 0.36 1.87 -4 -8 -16 1.85 2.09 5 8 16 2.59 1.98 5 8 16 -0.80 2.01 -5 -8 -16 3.06 2.05 -6 -8 -16 7.61 2.35 6 8 16 8.03 2.46 6 8 16 6.49 2.26 -7 -8 -16 20.99 3.08 7 8 16 20.13 2.95 7 8 16 11.25 2.60 8 8 16 -0.24 1.84 -8 -8 -16 2.84 2.03 8 8 16 1.05 1.95 9 8 16 5.89 2.20 -9 -8 -16 2.22 2.01 9 8 16 2.63 2.25 -10 -8 -16 5.76 2.42 10 8 16 5.09 2.48 10 8 16 7.24 2.30 11 8 16 4.17 2.08 11 8 16 0.97 2.11 12 8 16 3.14 2.07 12 8 16 1.13 1.94 -3 -9 -16 1.89 2.20 3 9 16 5.20 2.30 -4 -9 -16 1.25 2.04 4 9 16 -0.39 1.80 -5 -9 -16 -0.90 1.84 5 9 16 -0.93 2.00 6 9 16 -3.10 1.96 -6 -9 -16 3.52 2.32 7 9 16 16.64 2.96 7 9 16 10.39 2.44 -7 -9 -16 8.26 2.44 -8 -9 -16 12.13 2.66 8 9 16 8.40 2.26 8 9 16 9.94 2.67 -9 -9 -16 -0.80 1.98 9 9 16 3.62 2.16 9 9 16 -1.65 1.87 10 9 16 1.75 1.86 10 9 16 0.19 1.97 11 9 16 0.75 2.02 11 9 16 1.07 2.00 12 9 16 2.82 1.93 12 9 16 0.28 2.11 5 10 16 0.82 2.12 -5 -10 -16 -1.37 1.95 -6 -10 -16 0.45 2.18 6 10 16 -2.29 1.98 7 10 16 12.63 2.84 -7 -10 -16 8.93 2.54 7 10 16 7.27 2.27 8 10 16 -2.66 2.11 8 10 16 2.65 2.15 -8 -10 -16 -0.06 2.06 9 10 16 -1.12 1.67 9 10 16 1.79 2.14 10 10 16 -1.52 1.81 10 10 16 -2.10 1.79 11 10 16 4.58 2.26 11 10 16 2.51 2.28 12 10 16 0.11 2.24 12 10 16 2.17 2.20 -6 -11 -16 -0.98 2.00 6 11 16 2.05 2.30 7 11 16 5.03 2.33 -7 -11 -16 4.36 2.42 7 11 16 3.31 2.29 8 11 16 5.45 2.36 8 11 16 3.63 2.49 9 11 16 3.67 2.28 9 11 16 -0.92 1.91 10 11 16 1.64 2.25 10 11 16 -2.40 1.78 11 11 16 6.77 2.53 11 11 16 7.32 2.51 -4 2 -17 0.22 1.92 -2 1 -17 4.47 2.06 3 -1 17 -2.43 1.87 -3 1 -17 0.08 1.80 -4 1 -17 -0.87 1.82 4 -1 17 4.62 2.36 5 -1 17 2.64 2.27 -5 1 -17 0.67 1.89 -6 1 -17 -1.81 1.69 6 -1 17 1.51 2.03 -7 1 -17 8.34 2.42 2 0 17 0.22 1.88 -2 0 -17 1.02 1.92 -3 0 -17 2.10 1.98 3 0 17 0.11 1.99 4 0 17 2.52 2.03 -4 0 -17 -0.51 1.78 5 0 17 0.63 1.93 -5 0 -17 1.75 1.95 6 0 17 2.11 2.08 -6 0 -17 -0.71 1.71 6 0 17 -0.96 1.75 -7 0 -17 -0.02 1.93 -8 0 -17 5.72 2.39 -2 -1 -17 0.68 1.85 -3 -1 -17 3.05 2.02 3 1 17 -0.63 1.76 4 1 17 1.47 1.92 4 1 17 4.01 1.89 -4 -1 -17 -0.55 1.68 5 1 17 11.61 2.57 -5 -1 -17 15.79 2.76 5 1 17 12.68 2.71 6 1 17 7.27 2.46 6 1 17 13.52 2.65 -6 -1 -17 12.77 2.62 -7 -1 -17 0.87 1.90 7 1 17 1.73 1.96 -8 -1 -17 -3.20 1.71 8 1 17 -0.91 1.63 9 1 17 9.90 2.62 -9 -1 -17 5.53 2.53 -2 -2 -17 3.72 2.11 -3 -2 -17 -1.48 1.65 3 2 17 1.91 1.68 4 2 17 1.62 1.94 -4 -2 -17 3.72 2.13 4 2 17 -2.65 1.34 5 2 17 6.80 2.32 5 2 17 5.39 2.19 -5 -2 -17 7.59 2.41 6 2 17 20.90 3.10 -6 -2 -17 20.51 2.98 6 2 17 16.95 2.95 7 2 17 1.14 1.70 -7 -2 -17 -1.25 1.85 8 2 17 1.42 1.91 -8 -2 -17 2.27 2.12 9 2 17 1.50 1.87 -9 -2 -17 0.09 2.09 -10 -2 -17 1.55 2.30 -2 -3 -17 4.14 2.15 -3 -3 -17 4.33 2.22 3 3 17 1.15 1.89 4 3 17 0.63 1.59 -4 -3 -17 0.28 1.75 5 3 17 7.09 2.20 -5 -3 -17 1.27 1.94 5 3 17 0.83 1.78 -6 -3 -17 13.13 2.66 6 3 17 16.04 2.90 6 3 17 12.09 2.57 -7 -3 -17 0.44 1.80 7 3 17 2.60 1.88 8 3 17 3.60 1.98 -8 -3 -17 4.03 2.20 -9 -3 -17 4.57 2.27 9 3 17 3.60 2.07 10 3 17 2.27 2.19 -10 -3 -17 0.02 2.12 -2 -4 -17 -0.42 1.96 3 4 17 5.51 2.27 -3 -4 -17 -0.08 1.97 -4 -4 -17 12.22 2.63 4 4 17 8.67 2.46 5 4 17 -0.44 1.89 -5 -4 -17 3.45 2.06 6 4 17 3.06 1.98 -6 -4 -17 5.25 2.29 6 4 17 0.70 1.75 -7 -4 -17 2.17 2.13 7 4 17 0.53 1.81 -8 -4 -17 0.58 1.89 8 4 17 0.60 1.77 9 4 17 10.16 2.51 9 4 17 10.22 2.65 -9 -4 -17 9.51 2.66 -10 -4 -17 2.75 2.33 10 4 17 2.21 2.25 11 4 17 0.19 1.95 -11 -4 -17 -1.31 2.04 -2 -5 -17 1.71 2.07 -3 -5 -17 -4.85 1.58 4 5 17 9.82 2.45 -4 -5 -17 7.96 2.45 5 5 17 7.16 2.40 -5 -5 -17 5.27 2.12 6 5 17 0.53 1.88 -6 -5 -17 0.12 1.97 7 5 17 1.68 1.91 -7 -5 -17 3.17 2.25 8 5 17 -0.46 1.86 8 5 17 0.93 2.10 -8 -5 -17 2.22 2.26 9 5 17 -0.09 2.01 -9 -5 -17 1.28 2.11 10 5 17 3.20 2.33 -10 -5 -17 2.86 2.15 11 5 17 3.95 2.32 -11 -5 -17 -2.05 1.90 -3 -6 -17 1.47 1.97 -4 -6 -17 3.20 2.30 4 6 17 0.03 1.71 -5 -6 -17 1.40 1.95 5 6 17 5.97 2.24 -6 -6 -17 8.73 2.43 6 6 17 6.97 2.60 -7 -6 -17 5.94 2.38 7 6 17 -2.46 1.96 7 6 17 1.17 1.94 8 6 17 0.45 2.07 -8 -6 -17 2.76 2.25 8 6 17 -2.27 1.93 9 6 17 3.66 2.27 -9 -6 -17 3.32 2.10 10 6 17 19.64 3.06 -10 -6 -17 15.65 3.07 -11 -6 -17 6.16 2.50 11 6 17 6.58 2.24 11 6 17 9.68 2.61 -4 -7 -17 0.10 2.13 4 7 17 2.38 2.09 5 7 17 2.31 2.03 -5 -7 -17 -2.34 1.83 6 7 17 0.27 2.05 -6 -7 -17 4.29 2.31 7 7 17 7.38 2.44 -7 -7 -17 11.54 2.63 7 7 17 9.60 2.74 -8 -7 -17 1.56 2.06 8 7 17 -0.52 2.00 9 7 17 -4.62 1.66 -9 -7 -17 -3.33 1.63 10 7 17 4.77 2.50 10 7 17 2.57 2.08 -10 -7 -17 4.53 2.48 -11 -7 -17 0.62 2.15 11 7 17 3.67 2.13 11 7 17 -0.38 2.27 5 8 17 -0.03 2.03 -5 -8 -17 -0.22 2.04 -6 -8 -17 1.00 2.23 6 8 17 -2.08 2.06 -7 -8 -17 6.10 2.48 7 8 17 3.78 2.39 -8 -8 -17 5.02 2.45 8 8 17 4.20 2.41 -9 -8 -17 9.06 2.67 9 8 17 10.03 2.53 9 8 17 2.05 2.12 10 8 17 1.29 2.00 10 8 17 0.76 2.31 -10 -8 -17 3.19 2.24 11 8 17 0.52 2.18 11 8 17 0.16 2.02 -6 -9 -17 9.45 2.81 6 9 17 9.82 2.73 -7 -9 -17 -1.20 1.93 7 9 17 -0.17 2.18 8 9 17 1.23 2.26 -8 -9 -17 5.59 2.59 -9 -9 -17 15.68 3.00 9 9 17 15.24 2.69 9 9 17 5.78 2.65 10 9 17 6.82 2.64 10 9 17 9.00 2.49 -6 -2 -18 0.15 2.09 -5 -3 -18 4.96 2.35 -6 -3 -18 -0.76 2.12 6 3 18 -2.11 1.93 7 3 18 -3.05 1.82 -7 -3 -18 -1.97 1.99 -5 -4 -18 3.03 2.33 -6 -4 -18 -4.38 1.79 7 4 18 2.68 2.11 -7 -4 -18 1.66 2.27 7 4 18 -3.23 1.76 8 4 18 3.89 2.39 -8 -4 -18 0.68 2.11 -6 -5 -18 3.32 2.20 7 5 18 -2.23 1.94 -7 -5 -18 1.87 2.25 -8 -5 -18 5.81 2.58 8 5 18 9.46 2.85 -7 -6 -18 1.18 2.21 7 6 18 2.75 2.17 -8 -6 -18 4.38 2.47 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 4030 _shelx_res_file ; TITL in6 in P-1 shelx.res created by SHELXL-2018/3 at 16:26:13 on 06-Jun-2021 REM C17 1 0.666458 0.645515 0.046954 11.00000 0.05901 REM 0.20863 = 0.24284 -0.16558 0.02639 -0.04592 CELL 0.71073 10.6886 11.4878 11.8389 76.007 65.584 63.213 ZERR 2 0.0005 0.0005 0.0006 0.001 0.001 0.001 LATT 1 SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.003 0.002 = 11.5 0.77 12.011 SFAC H 0.493 10.511 0.323 26.126 0.14 3.142 0.041 57.8 0.003 0 0 0.62 0.32 = 1.008 SFAC N 12.213 0.006 3.132 9.893 2.013 28.998 1.166 0.583 -11.529 0.006 = 0.003 19.6 0.7 14.007 SFAC O 3.049 13.277 2.287 5.701 1.546 0.324 0.867 32.909 0.251 0.011 0.006 = 32.5 0.66 15.999 SFAC S 6.905 1.468 5.203 22.215 1.438 0.254 1.586 56.172 0.867 0.125 0.123 = 532 1.04 32.066 UNIT 44 56 2 12 6 SIZE 0.10 0.20 0.30 EQIV $1 -X,2-Y,-Z EQIV $2 -X,2-Y,1-Z DELU_SC 0.005 0.005 S3 > C22 SIMU_SC 0.005 0.01 2 S3 > C22 EADP C19_1 C19_2 EXYZ C19_1 C19_2 SAME_SC 0.001 0.04 S3 > C22 L.S. 99 PLAN -20 MPLA 6 S1 C1 C2 N1 C6 C7 MPLA 5 S2 C11 C12 C13 C14 HTAB C10 O2_$1 HTAB C2 O1_$2 HTAB C5 O1_$2 HTAB C6 O1_$2 BOND $H CONF fmap 2 acta MERG 2 OMIT -1 51 OMIT 0 0 1 OMIT 0 1 0 REM REM REM REM WGHT 0.090800 1.487500 WGHT 0.075800 0.538700 FVAR 0.78892 0.79234 S1 5 0.106429 0.885258 0.270141 11.00000 0.04415 0.03657 = 0.03971 -0.00170 -0.01502 -0.01506 S2 5 0.554565 0.970815 0.156981 11.00000 0.05365 0.06482 = 0.08174 -0.02666 -0.00057 -0.02871 O1 4 -0.031730 0.957524 0.361708 11.00000 0.04043 0.04701 = 0.05999 -0.00715 -0.01194 -0.01105 O2 4 0.103356 0.853855 0.162088 11.00000 0.08145 0.05792 = 0.04841 0.00443 -0.03116 -0.03727 O3 4 0.063181 1.205075 0.243682 11.00000 0.07955 0.03749 = 0.07987 -0.01212 -0.04357 -0.00575 O4 4 0.129798 1.114298 0.069715 11.00000 0.05673 0.05229 = 0.04163 0.00492 -0.01621 -0.01558 O5 4 0.376661 0.525425 0.287280 11.00000 0.07018 0.03721 = 0.08962 -0.00438 -0.01147 -0.00708 O6 4 0.411041 0.695425 0.163921 11.00000 0.06479 0.04410 = 0.05751 -0.01706 0.01041 -0.01502 N1 3 0.343109 0.847750 0.376703 11.00000 0.04001 0.03930 = 0.04263 -0.00652 -0.01334 -0.00973 AFIX 13 H1 2 0.426635 0.794818 0.309267 11.00000 -1.20000 AFIX 0 C1 1 0.199918 0.737892 0.352041 11.00000 0.04467 0.03629 = 0.03800 -0.00088 -0.01253 -0.01385 C2 1 0.239852 0.782356 0.441757 11.00000 0.04786 0.04357 = 0.03815 -0.00089 -0.01410 -0.01527 AFIX 13 H2 2 0.147318 0.843315 0.497164 11.00000 -1.20000 AFIX 0 C3 1 0.318782 0.670814 0.521519 11.00000 0.08427 0.06155 = 0.06257 0.01346 -0.04318 -0.02930 AFIX 23 H3A 2 0.246738 0.656734 0.600762 11.00000 -1.20000 H3B 2 0.375080 0.590302 0.479278 11.00000 -1.20000 AFIX 0 C4 1 0.420577 0.713982 0.539695 11.00000 0.09096 0.09788 = 0.09486 0.03678 -0.06194 -0.04870 AFIX 23 H4A 2 0.523656 0.652716 0.506363 11.00000 -1.20000 H4B 2 0.395321 0.719435 0.627467 11.00000 -1.20000 AFIX 0 C5 1 0.399900 0.847028 0.471265 11.00000 0.05083 0.06196 = 0.05877 -0.00615 -0.02765 -0.01446 AFIX 23 H5A 2 0.328281 0.916183 0.527048 11.00000 -1.20000 H5B 2 0.494141 0.857580 0.432665 11.00000 -1.20000 AFIX 0 C6 1 0.274215 0.979621 0.324759 11.00000 0.03822 0.03636 = 0.04033 -0.00867 -0.00994 -0.00948 AFIX 13 H6 2 0.187469 1.031597 0.391222 11.00000 -1.20000 AFIX 0 C7 1 0.222536 0.976566 0.222551 11.00000 0.04126 0.03434 = 0.03884 -0.00426 -0.01008 -0.01267 AFIX 13 H7 2 0.311127 0.937410 0.150506 11.00000 -1.20000 AFIX 0 C8 1 0.129208 1.113311 0.181959 11.00000 0.04461 0.03895 = 0.05003 0.00050 -0.01735 -0.01717 C9 1 0.030532 1.232623 0.022339 11.00000 0.07395 0.05929 = 0.06323 0.01512 -0.03333 -0.02081 AFIX 23 H9A 2 0.061777 1.230870 -0.066911 11.00000 -1.20000 H9B 2 0.037761 1.307949 0.038203 11.00000 -1.20000 AFIX 0 C10 1 -0.124986 1.245504 0.080627 11.00000 0.06718 0.11572 = 0.09643 -0.01737 -0.04178 -0.02193 AFIX 33 H10A 2 -0.187600 1.324389 0.047480 11.00000 -1.50000 H10B 2 -0.132705 1.171788 0.063818 11.00000 -1.50000 H10C 2 -0.156697 1.248790 0.168828 11.00000 -1.50000 AFIX 0 C11 1 0.384216 1.043504 0.269086 11.00000 0.04759 0.04256 = 0.04744 -0.00883 -0.01519 -0.01558 C12 1 0.367768 1.161700 0.296022 11.00000 0.06104 0.04586 = 0.05746 -0.00609 -0.02088 -0.02148 AFIX 43 H12 2 0.283730 1.216203 0.354333 11.00000 -1.20000 AFIX 0 C13 1 0.497371 1.187859 0.222007 11.00000 0.09597 0.06866 = 0.07248 -0.00912 -0.02921 -0.04963 AFIX 43 H13 2 0.506915 1.262846 0.227014 11.00000 -1.20000 AFIX 0 C14 1 0.604176 1.095410 0.144694 11.00000 0.07028 0.08453 = 0.07421 -0.01113 -0.01335 -0.04921 AFIX 43 H14 2 0.695061 1.098978 0.090502 11.00000 -1.20000 AFIX 0 C15 1 0.338428 0.640186 0.263865 11.00000 0.04851 0.03899 = 0.05024 -0.00696 -0.01404 -0.01308 C16 1 0.546711 0.609732 0.076020 11.00000 0.06895 0.07099 = 0.08525 -0.04165 0.01668 -0.02285 PART 1 AFIX 43 H16 2 0.549343 0.549916 0.033476 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H16A 2 0.524753 0.599733 0.008051 -21.00000 -1.20000 H16B 2 0.584819 0.524079 0.117016 -21.00000 -1.20000 AFIX 0 PART 0 C18 1 0.085595 0.676111 0.431245 11.00000 0.05580 0.04705 = 0.04081 0.00167 -0.01144 -0.02385 PART 1 AFIX 23 H18A 2 0.136028 0.596702 0.474240 21.00000 -1.20000 H18B 2 0.007236 0.735721 0.494289 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H18C 2 0.136028 0.596702 0.474240 -21.00000 -1.20000 H18D 2 0.007236 0.735721 0.494289 -21.00000 -1.20000 AFIX 0 RESI SC 1 PART 0 PART 1 S3 5 0.095826 0.503479 0.291299 21.00000 0.07482 0.04318 = 0.07337 -0.01248 -0.02132 -0.01994 C19 1 0.011654 0.642384 0.367762 21.00000 0.05619 0.04035 = 0.04270 0.00209 -0.01081 -0.02399 C20 1 -0.130978 0.704297 0.373139 21.00000 0.06371 0.05017 = 0.05688 -0.00299 -0.02285 -0.01535 AFIX 23 H20A 2 -0.148183 0.794177 0.341102 21.00000 -1.20000 H20B 2 -0.195416 0.705916 0.459804 21.00000 -1.20000 AFIX 0 C21 1 -0.064260 0.537754 0.263594 21.00000 0.06966 0.05527 = 0.06483 -0.00415 -0.02340 -0.02980 AFIX 43 H21 2 -0.071925 0.483193 0.222378 21.00000 -1.20000 AFIX 0 C22 1 -0.175673 0.649984 0.307040 21.00000 0.06572 0.06100 = 0.06050 -0.00093 -0.02144 -0.02669 AFIX 43 H22 2 -0.267612 0.686988 0.296132 21.00000 -1.20000 AFIX 0 RESI SC 2 PART 0 PART 2 S3 5 -0.164353 0.742185 0.368272 -21.00000 0.05883 0.05936 = 0.06880 0.00212 -0.02812 -0.02605 C19 1 0.011654 0.642384 0.367762 -21.00000 0.05619 0.04035 = 0.04270 0.00209 -0.01081 -0.02399 C20 1 0.067589 0.526440 0.321345 -21.00000 0.05736 0.04770 = 0.05127 0.00165 -0.01174 -0.03140 AFIX 43 H20 2 0.156587 0.459071 0.325815 -21.00000 -1.20000 AFIX 0 C21 1 -0.150421 0.617173 0.300847 -21.00000 0.06208 0.05494 = 0.06450 0.00252 -0.02313 -0.03050 AFIX 43 H21 2 -0.233728 0.621400 0.289946 -21.00000 -1.20000 AFIX 0 C22 1 -0.020596 0.514725 0.264434 -21.00000 0.06112 0.05054 = 0.05878 0.00228 -0.01856 -0.03223 AFIX 43 H22 2 0.006362 0.450567 0.213808 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C17 1 0.668878 0.627665 0.063652 21.00000 0.06602 0.21496 = 0.32756 -0.20109 0.01175 -0.03742 AFIX 137 H17A 2 0.756213 0.568897 0.005954 21.00000 -1.50000 H17B 2 0.680508 0.610621 0.142986 21.00000 -1.50000 H17C 2 0.656401 0.716174 0.033258 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C17A 1 0.661078 0.666929 0.026926 -21.00000 0.04310 0.05761 = 0.01756 -0.00850 0.01227 -0.02091 AFIX 137 H17D 2 0.625474 0.749063 -0.018241 -21.00000 -1.50000 H17E 2 0.752574 0.608189 -0.027517 -21.00000 -1.50000 H17F 2 0.678945 0.680424 0.094874 -21.00000 -1.50000 AFIX 0 HKLF 4 REM in6 in P-1 REM wR2 = 0.1342, GooF = S = 1.054, Restrained GooF = 1.071 for all data REM R1 = 0.0439 for 3774 Fo > 4sig(Fo) and 0.0509 for all 4375 data REM 337 parameters refined using 90 restraints END WGHT 0.0775 0.5288 REM Highest difference peak 0.325, deepest hole -0.563, 1-sigma level 0.051 Q1 1 0.5497 0.9607 0.2421 11.00000 0.05 0.33 Q2 1 0.3641 1.1644 0.3489 11.00000 0.05 0.30 Q3 1 0.3856 1.0996 0.3062 11.00000 0.05 0.29 Q4 1 0.5456 0.5172 0.1044 11.00000 0.05 0.29 Q5 1 0.5771 0.5749 0.1467 11.00000 0.05 0.28 Q6 1 0.1631 0.7999 0.3128 11.00000 0.05 0.25 Q7 1 0.5628 1.1150 0.2380 11.00000 0.05 0.24 Q8 1 0.2238 0.7606 0.3914 11.00000 0.05 0.24 Q9 1 -0.0216 0.6672 0.3598 11.00000 0.05 0.24 Q10 1 0.3974 1.1967 0.2726 11.00000 0.05 0.23 Q11 1 -0.2190 0.8149 0.4151 11.00000 0.05 0.23 Q12 1 0.3330 1.1715 0.2972 11.00000 0.05 0.23 Q13 1 0.4258 0.5605 0.2979 11.00000 0.05 0.23 Q14 1 0.4741 0.6759 0.5757 11.00000 0.05 0.22 Q15 1 0.0518 0.6570 0.3803 11.00000 0.05 0.22 Q16 1 0.2658 0.7010 0.3096 11.00000 0.05 0.21 Q17 1 0.2420 0.9819 0.2736 11.00000 0.05 0.20 Q18 1 0.1634 0.9382 0.2535 11.00000 0.05 0.20 Q19 1 0.4970 1.2170 0.2133 11.00000 0.05 0.20 Q20 1 0.5107 0.6499 -0.0239 11.00000 0.05 0.19 ; _shelx_res_checksum 98184 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 S S1 0.10643(6) 0.88526(5) 0.27014(5) 0.04061(16) Uani d 1 . . S S2 0.55456(8) 0.97081(7) 0.15698(7) 0.0688(2) Uani d 1 . . O O1 -0.03173(17) 0.95752(15) 0.36171(15) 0.0531(4) Uani d 1 . . O O2 0.1034(2) 0.85385(16) 0.16209(15) 0.0573(4) Uani d 1 . . O O3 0.0632(2) 1.20507(16) 0.24368(18) 0.0654(5) Uani d 1 . . O O4 0.12980(18) 1.11430(16) 0.06971(14) 0.0547(4) Uani d 1 . . O O5 0.3767(2) 0.52543(17) 0.2873(2) 0.0774(6) Uani d 1 . . O O6 0.4110(2) 0.69543(16) 0.16392(17) 0.0670(5) Uani d 1 . . N N1 0.34311(19) 0.84775(17) 0.37670(16) 0.0428(4) Uani d 1 . . H H1 0.426635 0.794818 0.309267 0.051 Uiso calc 1 . . C C1 0.1999(2) 0.73789(19) 0.35204(19) 0.0416(5) Uani d 1 . . C C2 0.2399(2) 0.7824(2) 0.44176(19) 0.0451(5) Uani d 1 . . H H2 0.147318 0.843315 0.497164 0.054 Uiso calc 1 . . C C3 0.3188(3) 0.6708(3) 0.5215(3) 0.0665(7) Uani d 1 . . H H3A 0.246738 0.656734 0.600762 0.080 Uiso calc 1 . . H H3B 0.375080 0.590302 0.479278 0.080 Uiso calc 1 . . C C4 0.4206(4) 0.7140(4) 0.5397(4) 0.0880(10) Uani d 1 . . H H4A 0.523656 0.652716 0.506363 0.106 Uiso calc 1 . . H H4B 0.395321 0.719435 0.627467 0.106 Uiso calc 1 . . C C5 0.3999(3) 0.8470(3) 0.4713(2) 0.0569(6) Uani d 1 . . H H5A 0.328281 0.916183 0.527048 0.068 Uiso calc 1 . . H H5B 0.494141 0.857580 0.432665 0.068 Uiso calc 1 . . C C6 0.2742(2) 0.97962(19) 0.32476(19) 0.0406(4) Uani d 1 . . H H6 0.187469 1.031597 0.391222 0.049 Uiso calc 1 . . C C7 0.2225(2) 0.97657(19) 0.22255(19) 0.0402(4) Uani d 1 . . H H7 0.311127 0.937410 0.150506 0.048 Uiso calc 1 . . C C8 0.1292(2) 1.1133(2) 0.1820(2) 0.0447(5) Uani d 1 . . C C9 0.0305(3) 1.2326(3) 0.0223(3) 0.0683(7) Uani d 1 . . H H9A 0.061777 1.230870 -0.066911 0.082 Uiso calc 1 . . H H9B 0.037761 1.307949 0.038203 0.082 Uiso calc 1 . . C C10 -0.1250(4) 1.2455(4) 0.0806(4) 0.0922(11) Uani d 1 . . H H10A -0.187600 1.324389 0.047480 0.138 Uiso calc 1 . . H H10B -0.132705 1.171788 0.063818 0.138 Uiso calc 1 . . H H10C -0.156697 1.248790 0.168828 0.138 Uiso calc 1 . . C C11 0.3842(2) 1.0435(2) 0.2691(2) 0.0462(5) Uani d 1 . . C C12 0.3678(3) 1.1617(2) 0.2960(2) 0.0542(6) Uani d 1 . . H H12 0.283730 1.216203 0.354333 0.065 Uiso calc 1 . . C C13 0.4974(4) 1.1879(3) 0.2220(3) 0.0715(8) Uani d 1 . . H H13 0.506915 1.262846 0.227014 0.086 Uiso calc 1 . . C C14 0.6042(3) 1.0954(3) 0.1447(3) 0.0721(8) Uani d 1 . . H H14 0.695061 1.098978 0.090502 0.087 Uiso calc 1 . . C C15 0.3384(3) 0.6402(2) 0.2639(2) 0.0481(5) Uani d 1 . . C C16 0.5467(4) 0.6097(3) 0.0760(3) 0.0857(10) Uani d 1 . . H H16 0.549343 0.549916 0.033476 0.103 Uiso calc 0.792(3) A 1 H H16A 0.524753 0.599733 0.008051 0.103 Uiso calc 0.208(3) A 2 H H16B 0.584819 0.524079 0.117016 0.103 Uiso calc 0.208(3) A 2 C C18 0.0856(3) 0.6761(2) 0.4312(2) 0.0494(5) Uani d 1 . . H H18A 0.136028 0.596702 0.474240 0.059 Uiso calc 0.792(3) A 1 H H18B 0.007236 0.735721 0.494289 0.059 Uiso calc 0.792(3) A 1 H H18C 0.136028 0.596702 0.474240 0.059 Uiso calc 0.208(3) A 2 H H18D 0.007236 0.735721 0.494289 0.059 Uiso calc 0.208(3) A 2 S S3_1 0.09583(14) 0.50348(10) 0.29130(11) 0.0652(4) Uani d 0.792(3) A 1 C C19_1 0.0117(2) 0.64238(18) 0.3678(2) 0.0478(5) Uani d 0.792(3) A 1 C C20_1 -0.1310(6) 0.7043(5) 0.3731(7) 0.0594(11) Uani d 0.792(3) A 1 H H20A_1 -0.148183 0.794177 0.341102 0.071 Uiso calc 0.792(3) A 1 H H20B_1 -0.195416 0.705916 0.459804 0.071 Uiso calc 0.792(3) A 1 C C21_1 -0.0643(5) 0.5378(4) 0.2636(5) 0.0613(9) Uani d 0.792(3) A 1 H H21_1 -0.071925 0.483193 0.222378 0.074 Uiso calc 0.792(3) A 1 C C22_1 -0.1757(5) 0.6500(4) 0.3070(5) 0.0627(9) Uani d 0.792(3) A 1 H H22_1 -0.267612 0.686988 0.296132 0.075 Uiso calc 0.792(3) A 1 S S3_2 -0.1644(4) 0.7422(5) 0.3683(7) 0.0605(12) Uani d 0.208(3) A 2 C C19_2 0.0117(2) 0.64238(18) 0.3678(2) 0.0478(5) Uani d 0.208(3) A 2 C C20_2 0.0676(16) 0.5264(9) 0.3213(15) 0.052(2) Uani d 0.208(3) A 2 H H20_2 0.156587 0.459071 0.325815 0.062 Uiso calc 0.208(3) A 2 C C21_2 -0.1504(17) 0.6172(13) 0.301(2) 0.059(2) Uani d 0.208(3) A 2 H H21_2 -0.233728 0.621400 0.289946 0.070 Uiso calc 0.208(3) A 2 C C22_2 -0.0206(14) 0.5147(15) 0.2644(17) 0.055(2) Uani d 0.208(3) A 2 H H22_2 0.006362 0.450567 0.213808 0.066 Uiso calc 0.208(3) A 2 C C17_2 0.6689(10) 0.6277(11) 0.0637(12) 0.203(6) Uani d 0.792(3) A 1 H H17A_2 0.756213 0.568897 0.005954 0.305 Uiso calc 0.792(3) A 1 H H17B_2 0.680508 0.610621 0.142986 0.305 Uiso calc 0.792(3) A 1 H H17C_2 0.656401 0.716174 0.033258 0.305 Uiso calc 0.792(3) A 1 C C17A_2 0.661(2) 0.6669(18) 0.0269(11) 0.046(3) Uani d 0.208(3) A 2 H H17D_2 0.625474 0.749063 -0.018241 0.069 Uiso calc 0.208(3) A 2 H H17E_2 0.752574 0.608189 -0.027517 0.069 Uiso calc 0.208(3) A 2 H H17F_2 0.678945 0.680424 0.094874 0.069 Uiso calc 0.208(3) A 2 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 S1 0.0442(3) 0.0366(3) 0.0397(3) -0.0151(2) -0.0150(2) -0.0017(2) S2 0.0537(4) 0.0648(4) 0.0817(5) -0.0287(3) -0.0006(3) -0.0267(4) O1 0.0404(8) 0.0470(9) 0.0600(10) -0.0110(7) -0.0119(7) -0.0071(7) O2 0.0814(12) 0.0579(10) 0.0484(9) -0.0373(9) -0.0312(8) 0.0044(7) O3 0.0795(12) 0.0375(9) 0.0799(12) -0.0058(8) -0.0436(10) -0.0121(8) O4 0.0567(10) 0.0523(9) 0.0416(8) -0.0156(8) -0.0162(7) 0.0049(7) O5 0.0702(12) 0.0372(9) 0.0896(14) -0.0071(8) -0.0115(10) -0.0044(9) O6 0.0648(11) 0.0441(9) 0.0575(10) -0.0150(8) 0.0104(8) -0.0171(8) N1 0.0400(9) 0.0393(9) 0.0426(9) -0.0097(7) -0.0133(7) -0.0065(7) C1 0.0447(11) 0.0363(10) 0.0380(10) -0.0139(9) -0.0125(9) -0.0009(8) C2 0.0479(12) 0.0436(11) 0.0382(10) -0.0153(9) -0.0141(9) -0.0009(8) C3 0.0843(19) 0.0615(16) 0.0626(16) -0.0293(14) -0.0432(15) 0.0135(12) C4 0.091(2) 0.098(2) 0.095(2) -0.049(2) -0.062(2) 0.0368(19) C5 0.0508(13) 0.0620(15) 0.0588(14) -0.0145(11) -0.0276(11) -0.0061(11) C6 0.0382(10) 0.0364(10) 0.0403(10) -0.0095(8) -0.0099(8) -0.0087(8) C7 0.0413(10) 0.0343(10) 0.0388(10) -0.0127(8) -0.0101(8) -0.0043(8) C8 0.0446(11) 0.0389(11) 0.0500(12) -0.0172(9) -0.0174(9) 0.0005(9) C9 0.0739(18) 0.0593(15) 0.0632(16) -0.0208(13) -0.0333(14) 0.0151(12) C10 0.0672(19) 0.116(3) 0.096(2) -0.0219(19) -0.0418(18) -0.017(2) C11 0.0476(12) 0.0426(11) 0.0474(12) -0.0156(9) -0.0152(10) -0.0088(9) C12 0.0610(14) 0.0459(12) 0.0575(14) -0.0215(11) -0.0209(11) -0.0061(10) C13 0.096(2) 0.0687(17) 0.0725(18) -0.0496(17) -0.0292(16) -0.0091(14) C14 0.0703(17) 0.085(2) 0.0742(18) -0.0492(16) -0.0134(14) -0.0111(15) C15 0.0485(12) 0.0390(11) 0.0502(12) -0.0131(9) -0.0140(10) -0.0070(9) C16 0.0689(19) 0.0710(19) 0.085(2) -0.0228(15) 0.0167(16) -0.0416(16) C18 0.0558(13) 0.0470(12) 0.0408(11) -0.0238(10) -0.0114(10) 0.0017(9) S3_1 0.0748(7) 0.0432(5) 0.0734(8) -0.0199(5) -0.0213(6) -0.0125(4) C19_1 0.0562(12) 0.0403(10) 0.0427(10) -0.0240(9) -0.0108(9) 0.0021(8) C20_1 0.064(2) 0.050(2) 0.057(2) -0.0153(16) -0.0229(19) -0.0030(19) C21_1 0.070(2) 0.055(2) 0.0648(18) -0.0298(17) -0.0234(18) -0.0042(15) C22_1 0.066(2) 0.061(2) 0.0605(19) -0.0267(16) -0.0214(17) -0.0009(18) S3_2 0.059(2) 0.059(3) 0.069(2) -0.0261(17) -0.0281(19) 0.002(2) C19_2 0.0562(12) 0.0403(10) 0.0427(10) -0.0240(9) -0.0108(9) 0.0021(8) C20_2 0.057(3) 0.048(3) 0.051(4) -0.031(3) -0.012(3) 0.002(3) C21_2 0.062(4) 0.055(4) 0.065(4) -0.030(3) -0.023(3) 0.003(3) C22_2 0.061(4) 0.051(4) 0.059(4) -0.032(3) -0.019(4) 0.002(3) C17_2 0.066(4) 0.215(11) 0.328(15) -0.037(6) 0.012(7) -0.201(11) C17A_2 0.043(7) 0.058(7) 0.018(4) -0.021(6) 0.012(4) -0.009(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 '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 O2 S1 O1 . . 119.13(11) ? O2 S1 C7 . . 109.00(10) ? O1 S1 C7 . . 106.71(10) ? O2 S1 C1 . . 110.41(10) ? O1 S1 C1 . . 106.16(10) ? C7 S1 C1 . . 104.40(10) ? C14 S2 C11 . . 92.13(13) ? C8 O4 C9 . . 117.8(2) ? C15 O6 C16 . . 117.5(2) ? C6 N1 C2 . . 113.82(16) ? C6 N1 C5 . . 112.22(17) ? C2 N1 C5 . . 104.09(17) ? C6 N1 H1 . . 108.8 ? C2 N1 H1 . . 108.8 ? C5 N1 H1 . . 108.8 ? C15 C1 C18 . . 110.35(17) ? C15 C1 C2 . . 111.72(18) ? C18 C1 C2 . . 108.07(17) ? C15 C1 S1 . . 112.48(14) ? C18 C1 S1 . . 107.65(15) ? C2 C1 S1 . . 106.34(14) ? N1 C2 C3 . . 103.90(19) ? N1 C2 C1 . . 112.87(16) ? C3 C2 C1 . . 114.40(19) ? N1 C2 H2 . . 108.5 ? C3 C2 H2 . . 108.5 ? C1 C2 H2 . . 108.5 ? C4 C3 C2 . . 105.1(2) ? C4 C3 H3A . . 110.7 ? C2 C3 H3A . . 110.7 ? C4 C3 H3B . . 110.7 ? C2 C3 H3B . . 110.7 ? H3A C3 H3B . . 108.8 ? C3 C4 C5 . . 106.6(2) ? C3 C4 H4A . . 110.4 ? C5 C4 H4A . . 110.4 ? C3 C4 H4B . . 110.4 ? C5 C4 H4B . . 110.4 ? H4A C4 H4B . . 108.6 ? N1 C5 C4 . . 103.6(2) ? N1 C5 H5A . . 111.0 ? C4 C5 H5A . . 111.0 ? N1 C5 H5B . . 111.0 ? C4 C5 H5B . . 111.0 ? H5A C5 H5B . . 109.0 ? N1 C6 C11 . . 110.30(17) ? N1 C6 C7 . . 110.96(16) ? C11 C6 C7 . . 108.32(17) ? N1 C6 H6 . . 109.1 ? C11 C6 H6 . . 109.1 ? C7 C6 H6 . . 109.1 ? C8 C7 C6 . . 111.47(16) ? C8 C7 S1 . . 105.56(14) ? C6 C7 S1 . . 113.68(14) ? C8 C7 H7 . . 108.7 ? C6 C7 H7 . . 108.7 ? S1 C7 H7 . . 108.7 ? O3 C8 O4 . . 125.3(2) ? O3 C8 C7 . . 124.6(2) ? O4 C8 C7 . . 110.05(18) ? O4 C9 C10 . . 111.5(2) ? O4 C9 H9A . . 109.3 ? C10 C9 H9A . . 109.3 ? O4 C9 H9B . . 109.3 ? C10 C9 H9B . . 109.3 ? H9A C9 H9B . . 108.0 ? C9 C10 H10A . . 109.5 ? C9 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C9 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? C12 C11 C6 . . 128.0(2) ? C12 C11 S2 . . 111.20(18) ? C6 C11 S2 . . 120.78(15) ? C11 C12 C13 . . 110.5(2) ? C11 C12 H12 . . 124.7 ? C13 C12 H12 . . 124.7 ? C14 C13 C12 . . 114.2(2) ? C14 C13 H13 . . 122.9 ? C12 C13 H13 . . 122.9 ? C13 C14 S2 . . 112.0(2) ? C13 C14 H14 . . 124.0 ? S2 C14 H14 . . 124.0 ? O5 C15 O6 . . 124.4(2) ? O5 C15 C1 . . 121.9(2) ? O6 C15 C1 . . 113.64(18) ? C17_2 C16 O6 . . 111.8(4) ? O6 C16 C17A_2 . . 109.3(7) ? C17_2 C16 H16 . . 124.1 ? O6 C16 H16 . . 124.1 ? O6 C16 H16A . . 109.8 ? C17A_2 C16 H16A . . 109.8 ? O6 C16 H16B . . 109.8 ? C17A_2 C16 H16B . . 109.8 ? H16A C16 H16B . . 108.3 ? C19_2 C18 C1 . . 118.81(18) ? C19_1 C18 C1 . . 118.81(18) ? C19_1 C18 H18A . . 107.6 ? C1 C18 H18A . . 107.6 ? C19_1 C18 H18B . . 107.6 ? C1 C18 H18B . . 107.6 ? H18A C18 H18B . . 107.0 ? C19_2 C18 H18C . . 107.6 ? C1 C18 H18C . . 107.6 ? C19_2 C18 H18D . . 107.6 ? C1 C18 H18D . . 107.6 ? H18C C18 H18D . . 107.0 ? C19_1 S3_1 C21_1 . . 91.52(18) ? C20_1 C19_1 C18 . . 127.1(3) ? C20_1 C19_1 S3_1 . . 109.6(3) ? C18 C19_1 S3_1 . . 122.94(17) ? C19_1 C20_1 C22_1 . . 116.2(5) ? C19_1 C20_1 H20A_1 . . 108.2 ? C22_1 C20_1 H20A_1 . . 108.2 ? C19_1 C20_1 H20B_1 . . 108.2 ? C22_1 C20_1 H20B_1 . . 108.2 ? H20A_1 C20_1 H20B_1 . . 107.4 ? C22_1 C21_1 S3_1 . . 113.4(4) ? C22_1 C21_1 H21_1 . . 123.3 ? S3_1 C21_1 H21_1 . . 123.3 ? C21_1 C22_1 C20_1 . . 109.0(5) ? C21_1 C22_1 H22_1 . . 125.5 ? C20_1 C22_1 H22_1 . . 125.5 ? C19_2 S3_2 C21_2 . . 85.3(6) ? C20_2 C19_2 C18 . . 123.6(7) ? C20_2 C19_2 S3_2 . . 114.4(6) ? C18 C19_2 S3_2 . . 121.4(3) ? C19_2 C20_2 C22_2 . . 114.6(11) ? C19_2 C20_2 H20_2 . . 122.7 ? C22_2 C20_2 H20_2 . . 122.7 ? C22_2 C21_2 S3_2 . . 120.2(12) ? C22_2 C21_2 H21_2 . . 119.9 ? S3_2 C21_2 H21_2 . . 119.9 ? C21_2 C22_2 C20_2 . . 103.9(13) ? C21_2 C22_2 H22_2 . . 128.1 ? C20_2 C22_2 H22_2 . . 128.1 ? C16 C17_2 H17A_2 . . 109.5 ? C16 C17_2 H17B_2 . . 109.5 ? H17A_2 C17_2 H17B_2 . . 109.5 ? C16 C17_2 H17C_2 . . 109.5 ? H17A_2 C17_2 H17C_2 . . 109.5 ? H17B_2 C17_2 H17C_2 . . 109.5 ? C16 C17A_2 H17D_2 . . 109.5 ? C16 C17A_2 H17E_2 . . 109.5 ? H17D_2 C17A_2 H17E_2 . . 109.5 ? C16 C17A_2 H17F_2 . . 109.5 ? H17D_2 C17A_2 H17F_2 . . 109.5 ? H17E_2 C17A_2 H17F_2 . . 109.5 ? 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 S1 O2 . 1.4270(17) ? S1 O1 . 1.4324(16) ? S1 C7 . 1.808(2) ? S1 C1 . 1.813(2) ? S2 C14 . 1.694(3) ? S2 C11 . 1.715(2) ? O3 C8 . 1.191(3) ? O4 C8 . 1.324(3) ? O4 C9 . 1.453(3) ? O5 C15 . 1.189(3) ? O6 C15 . 1.314(3) ? O6 C16 . 1.455(3) ? N1 C6 . 1.461(3) ? N1 C2 . 1.463(3) ? N1 C5 . 1.475(3) ? N1 H1 . 0.9800 ? C1 C15 . 1.527(3) ? C1 C18 . 1.546(3) ? C1 C2 . 1.551(3) ? C2 C3 . 1.531(3) ? C2 H2 . 0.9800 ? C3 C4 . 1.486(4) ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.512(4) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 C11 . 1.503(3) ? C6 C7 . 1.537(3) ? C6 H6 . 0.9800 ? C7 C8 . 1.521(3) ? C7 H7 . 0.9800 ? C9 C10 . 1.463(4) ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 H10A . 0.9600 ? C10 H10B . 0.9600 ? C10 H10C . 0.9600 ? C11 C12 . 1.387(3) ? C12 C13 . 1.422(4) ? C12 H12 . 0.9300 ? C13 C14 . 1.335(4) ? C13 H13 . 0.9300 ? C14 H14 . 0.9300 ? C16 C17_2 . 1.356(10) ? C16 C17A_2 . 1.489(19) ? C16 H16 . 0.9300 ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C18 C19_2 . 1.499(3) ? C18 C19_1 . 1.499(3) ? C18 H18A . 0.9700 ? C18 H18B . 0.9700 ? C18 H18C . 0.9700 ? C18 H18D . 0.9700 ? S3_1 C19_1 . 1.705(2) ? S3_1 C21_1 . 1.728(4) ? C19_1 C20_1 . 1.341(6) ? C20_1 C22_1 . 1.430(7) ? C20_1 H20A_1 . 0.9700 ? C20_1 H20B_1 . 0.9700 ? C21_1 C22_1 . 1.332(5) ? C21_1 H21_1 . 0.9300 ? C22_1 H22_1 . 0.9300 ? S3_2 C19_2 . 1.704(2) ? S3_2 C21_2 . 1.728(4) ? C19_2 C20_2 . 1.341(6) ? C20_2 C22_2 . 1.430(7) ? C20_2 H20_2 . 0.9300 ? C21_2 C22_2 . 1.332(5) ? C21_2 H21_2 . 0.9300 ? C22_2 H22_2 . 0.9300 ? C17_2 H17A_2 . 0.9600 ? C17_2 H17B_2 . 0.9600 ? C17_2 H17C_2 . 0.9600 ? C17A_2 H17D_2 . 0.9600 ? C17A_2 H17E_2 . 0.9600 ? C17A_2 H17F_2 . 0.9600 ? 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 C10 H10B O2 2_575 0.96 2.63 3.227(4) 120.3 yes C2 H2 O1 2_576 0.98 2.67 3.519(3) 144.7 yes C5 H5A O1 2_576 0.97 2.69 3.491(3) 140.7 yes C6 H6 O1 2_576 0.98 2.70 3.560(3) 146.3 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 O2 S1 C1 C15 . . . . 40.84(18) ? O1 S1 C1 C15 . . . . 171.28(15) ? C7 S1 C1 C15 . . . . -76.17(17) ? O2 S1 C1 C18 . . . . -80.94(16) ? O1 S1 C1 C18 . . . . 49.50(17) ? C7 S1 C1 C18 . . . . 162.05(14) ? O2 S1 C1 C2 . . . . 163.44(14) ? O1 S1 C1 C2 . . . . -66.12(16) ? C7 S1 C1 C2 . . . . 46.43(16) ? C6 N1 C2 C3 . . . . -162.13(19) ? C5 N1 C2 C3 . . . . -39.6(2) ? C6 N1 C2 C1 . . . . 73.4(2) ? C5 N1 C2 C1 . . . . -164.14(18) ? C15 C1 C2 N1 . . . . 60.9(2) ? C18 C1 C2 N1 . . . . -177.54(17) ? S1 C1 C2 N1 . . . . -62.20(19) ? C15 C1 C2 C3 . . . . -57.7(3) ? C18 C1 C2 C3 . . . . 63.9(2) ? S1 C1 C2 C3 . . . . 179.27(18) ? N1 C2 C3 C4 . . . . 24.3(3) ? C1 C2 C3 C4 . . . . 147.8(2) ? C2 C3 C4 C5 . . . . -0.2(4) ? C6 N1 C5 C4 . . . . 163.0(2) ? C2 N1 C5 C4 . . . . 39.5(3) ? C3 C4 C5 N1 . . . . -23.8(3) ? C2 N1 C6 C11 . . . . 175.34(17) ? C5 N1 C6 C11 . . . . 57.4(2) ? C2 N1 C6 C7 . . . . -64.6(2) ? C5 N1 C6 C7 . . . . 177.47(18) ? N1 C6 C7 C8 . . . . 171.04(16) ? C11 C6 C7 C8 . . . . -67.7(2) ? N1 C6 C7 S1 . . . . 51.9(2) ? C11 C6 C7 S1 . . . . 173.09(13) ? O2 S1 C7 C8 . . . . 75.37(16) ? O1 S1 C7 C8 . . . . -54.49(16) ? C1 S1 C7 C8 . . . . -166.65(14) ? O2 S1 C7 C6 . . . . -162.15(14) ? O1 S1 C7 C6 . . . . 67.99(16) ? C1 S1 C7 C6 . . . . -44.17(16) ? C9 O4 C8 O3 . . . . -6.6(3) ? C9 O4 C8 C7 . . . . 172.04(19) ? C6 C7 C8 O3 . . . . -22.8(3) ? S1 C7 C8 O3 . . . . 101.0(2) ? C6 C7 C8 O4 . . . . 158.49(17) ? S1 C7 C8 O4 . . . . -77.62(19) ? C8 O4 C9 C10 . . . . -75.7(3) ? N1 C6 C11 C12 . . . . -124.6(2) ? C7 C6 C11 C12 . . . . 113.8(3) ? N1 C6 C11 S2 . . . . 55.8(2) ? C7 C6 C11 S2 . . . . -65.8(2) ? C14 S2 C11 C12 . . . . -0.3(2) ? C14 S2 C11 C6 . . . . 179.4(2) ? C6 C11 C12 C13 . . . . -179.5(2) ? S2 C11 C12 C13 . . . . 0.2(3) ? C11 C12 C13 C14 . . . . -0.1(4) ? C12 C13 C14 S2 . . . . -0.1(4) ? C11 S2 C14 C13 . . . . 0.2(3) ? C16 O6 C15 O5 . . . . 0.4(4) ? C16 O6 C15 C1 . . . . 178.5(2) ? C18 C1 C15 O5 . . . . -27.1(3) ? C2 C1 C15 O5 . . . . 93.1(3) ? S1 C1 C15 O5 . . . . -147.4(2) ? C18 C1 C15 O6 . . . . 154.7(2) ? C2 C1 C15 O6 . . . . -85.0(2) ? S1 C1 C15 O6 . . . . 34.5(3) ? C15 O6 C16 C17_2 . . . . -118.1(7) ? C15 O6 C16 C17A_2 . . . . -141.0(7) ? C15 C1 C18 C19_2 . . . . -66.3(2) ? C2 C1 C18 C19_2 . . . . 171.31(19) ? S1 C1 C18 C19_2 . . . . 56.8(2) ? C15 C1 C18 C19_1 . . . . -66.3(2) ? C2 C1 C18 C19_1 . . . . 171.31(19) ? S1 C1 C18 C19_1 . . . . 56.8(2) ? C1 C18 C19_1 C20_1 . . . . -107.6(4) ? C1 C18 C19_1 S3_1 . . . . 80.6(2) ? C21_1 S3_1 C19_1 C20_1 . . . . 2.3(4) ? C21_1 S3_1 C19_1 C18 . . . . 175.3(3) ? C18 C19_1 C20_1 C22_1 . . . . -178.0(4) ? S3_1 C19_1 C20_1 C22_1 . . . . -5.4(7) ? C19_1 S3_1 C21_1 C22_1 . . . . 1.4(4) ? S3_1 C21_1 C22_1 C20_1 . . . . -4.4(7) ? C19_1 C20_1 C22_1 C21_1 . . . . 6.4(8) ? C1 C18 C19_2 C20_2 . . . . 89.6(9) ? C1 C18 C19_2 S3_2 . . . . -99.5(3) ? C21_2 S3_2 C19_2 C20_2 . . . . -0.9(13) ? C21_2 S3_2 C19_2 C18 . . . . -172.5(8) ? C18 C19_2 C20_2 C22_2 . . . . -179.9(11) ? S3_2 C19_2 C20_2 C22_2 . . . . 8.6(17) ? C19_2 S3_2 C21_2 C22_2 . . . . -8.0(19) ? S3_2 C21_2 C22_2 C20_2 . . . . 13(2) ? C19_2 C20_2 C22_2 C21_2 . . . . -13(2) ? _cod_database_fobs_code 2243862