#------------------------------------------------------------------------------ #$Date: 2022-08-10 02:41:57 +0100 (Wed, 10 Aug 2022) $ #$Revision: 277183 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244141.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_2244141 loop_ _publ_author_name 'Mohamed, Shaaban K.' 'Mague, Joel T.' 'Akkurt, Mehmet' 'Alfayomy, Abdallah M.' 'Ragab, Fatma A. F.' 'Abd ul-Malik, Mokhtar A.' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of ethyl (3E)-5-(4-fluorophenyl)3-{[(4-methoxyphenyl)formamido]imino}-7-methyl-2H,3H,5H-[1,3]thiazolo[3,2-a]pyrimidine-6-carboxylate 0.25-hydrate ; _journal_coeditor_code WM5648 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022006041 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C24 H23 F N4 O4 S, 0.25H2 O' _chemical_formula_moiety 'C24 H23 F N4 O4 S, 0.25(H2 O)' _chemical_formula_sum 'C24 H23.5 F N4 O4.25 S' _chemical_formula_weight 487.032 _chemical_name_systematic ;Ethyl (3E)-5-(4-fluorophenyl)3-{[(4-methoxyphenyl)formamido]imino}-7-methyl-2H,3H,5H-[1,3]thiazolo[3,2-a]pyrimidine-6-carboxylate 0.25-hydrate ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/1 _cell_angle_alpha 90 _cell_angle_beta 109.9410(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.4316(3) _cell_length_b 10.8518(2) _cell_length_c 15.5940(3) _cell_measurement_reflns_used 9970 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 74.4266 _cell_measurement_theta_min 3.2576 _cell_volume 2295.74(8) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Bruker D8 VENTURE PHOTON 100 CMOS' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_unetI/netI 0.0253 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 17597 _diffrn_reflns_theta_full 69.000 _diffrn_reflns_theta_max 74.419 _diffrn_reflns_theta_min 3.258 _diffrn_source 'INCOATEC I\mS micro--focus source' _exptl_absorpt_coefficient_mu 1.677 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1018 _exptl_crystal_size_max 0.147 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.110 _refine_diff_density_max 0.341 _refine_diff_density_min -0.556 _refine_ls_extinction_coef 0.00229(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL-2018/1 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 409 _refine_ls_number_reflns 4576 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0349 _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^)+(0.0389P)^2^+1.1637P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.0881 _reflns_number_gt 4142 _reflns_number_total 4576 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5648sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244141 _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 0.791 _shelx_estimated_absorpt_t_max 0.837 _shelx_hkl_file ; -1 0 0 1787.02 51.09 1 0 0 1652.83 51.29 2 0 0 150.68 4.80 -2 0 0 163.28 4.80 -3 0 0 2107.19 62.79 3 0 0 2078.79 62.79 4 0 0 2432.16 72.69 5 0 0 760.52 23.20 -5 0 0 789.52 23.30 6 0 0 995.20 29.60 -6 0 0 978.20 29.70 7 0 0 44.70 2.10 -9 0 0 235.48 7.80 -9 0 0 238.68 7.90 -9 0 0 229.78 7.70 -10 0 0 170.38 6.00 -10 0 0 176.78 6.20 -10 0 0 177.58 6.10 -11 0 0 185.98 6.50 -11 0 0 189.38 6.60 -12 0 0 261.07 8.90 -12 0 0 274.07 9.00 -13 0 0 65.19 2.90 -13 0 0 64.79 3.00 -14 0 0 52.99 2.50 14 0 0 53.59 2.50 -15 0 0 153.18 5.20 15 0 0 155.58 5.20 -15 0 0 151.98 5.30 -16 0 0 28.20 1.50 0 -1 0 0.00 0.10 0 1 0 0.10 0.10 1 -1 0 511.55 15.70 -1 -1 0 548.75 15.80 1 1 0 504.45 15.60 -2 -1 0 212.38 6.60 2 -1 0 216.68 6.60 -2 1 0 223.28 6.60 2 1 0 212.88 6.50 3 -1 0 446.66 13.90 -3 -1 0 482.65 13.90 -3 1 0 481.15 13.90 3 1 0 446.36 13.90 -4 -1 0 1994.80 58.89 4 -1 0 1962.70 59.19 -4 1 0 1937.41 58.79 4 1 0 1965.00 59.49 5 -1 0 326.97 10.10 -5 -1 0 321.37 10.10 5 1 0 328.07 10.10 -5 1 0 331.47 10.10 -6 -1 0 104.69 3.80 6 -1 0 108.49 3.80 6 1 0 109.39 3.70 -6 1 0 109.79 3.90 7 -1 0 889.61 26.90 7 1 0 886.61 26.80 8 -1 0 220.28 7.40 8 1 0 211.58 7.30 -9 -1 0 1.50 0.80 -9 -1 0 1.10 0.90 -9 -1 0 6.90 1.90 -9 1 0 -0.30 0.90 -9 1 0 1.30 0.90 -10 -1 0 3.20 0.90 -10 -1 0 3.80 0.90 -10 -1 0 6.40 1.90 -10 1 0 3.00 0.90 -10 1 0 3.80 0.90 -11 -1 0 57.79 2.80 -11 -1 0 64.29 3.10 -11 -1 0 57.99 2.70 -11 1 0 64.89 2.90 -11 1 0 59.99 2.80 -12 -1 0 214.28 7.50 -12 -1 0 225.18 7.50 -12 1 0 217.58 7.50 -12 1 0 218.98 7.50 13 -1 0 47.10 2.40 -13 -1 0 45.50 2.40 -13 -1 0 45.00 2.50 -13 1 0 47.00 2.50 -13 1 0 49.00 2.40 -14 -1 0 166.58 6.70 14 -1 0 174.58 5.90 -14 -1 0 174.18 6.00 -14 1 0 183.68 6.10 -14 1 0 169.98 6.00 -15 -1 0 104.99 4.00 15 1 0 102.09 3.80 -15 1 0 111.59 3.90 -15 1 0 110.59 3.90 -16 -1 0 140.19 4.60 -16 1 0 129.19 4.50 -16 1 0 130.09 4.50 0 2 0 385.66 11.60 1 -2 0 815.72 24.50 -1 2 0 823.82 24.60 -2 -2 0 11.80 0.60 2 -2 0 11.90 0.60 -2 2 0 10.50 0.60 2 2 0 9.30 0.50 -3 -2 0 854.41 24.80 3 -2 0 744.33 25.00 -3 2 0 839.52 24.70 3 2 0 879.81 25.00 4 -2 0 2.20 0.50 -4 2 0 1.80 0.50 4 2 0 1.30 0.40 -5 -2 0 183.08 5.90 5 2 0 173.88 5.80 -5 2 0 182.28 5.80 6 -2 0 65.59 2.60 -6 -2 0 60.89 2.60 6 2 0 65.59 2.50 -6 2 0 57.89 2.60 7 -2 0 243.58 8.40 7 -2 0 264.37 8.50 7 2 0 268.87 8.40 -8 -2 0 118.19 4.30 -8 -2 0 117.79 4.30 -9 -2 0 143.39 4.90 -9 -2 0 142.79 5.00 -9 -2 0 131.19 5.00 -9 2 0 137.79 5.00 -10 -2 0 36.90 2.60 -10 -2 0 35.90 2.10 -10 -2 0 34.20 1.90 -10 -2 0 35.60 2.20 -10 2 0 35.30 2.10 -10 2 0 36.80 2.20 11 -2 0 4.20 1.10 -11 -2 0 6.50 2.10 -11 -2 0 8.50 1.60 -11 -2 0 4.40 1.10 -11 -2 0 2.30 0.90 -11 2 0 6.10 1.30 -11 2 0 4.40 1.30 -12 -2 0 187.38 6.60 -12 -2 0 188.48 6.60 -12 -2 0 186.88 6.40 12 -2 0 196.28 6.50 -12 2 0 179.18 6.60 -12 2 0 192.48 6.60 13 -2 0 71.39 3.10 -13 -2 0 70.59 3.10 -13 2 0 72.29 3.10 -13 2 0 73.69 3.20 -14 -2 0 8.10 1.10 -14 2 0 7.90 1.30 -14 2 0 12.20 1.30 -15 -2 0 13.20 1.30 -15 2 0 13.60 1.20 -15 2 0 13.70 1.20 -16 -2 0 2.20 0.50 -16 2 0 1.20 0.70 -16 2 0 2.20 0.70 0 3 0 -0.10 0.20 1 -3 0 56.99 2.10 1 3 0 57.29 2.10 1 3 0 55.19 2.00 2 -3 0 0.50 0.20 -2 3 0 -0.10 0.20 2 3 0 0.10 0.20 3 -3 0 96.39 3.70 3 3 0 108.49 3.50 -3 3 0 104.59 3.50 4 -3 0 1083.89 32.90 -4 -3 0 1143.29 32.90 -4 3 0 1085.09 32.80 4 3 0 1083.49 32.80 -5 -3 0 0.80 0.50 5 -3 0 2.10 0.70 5 -3 0 1.60 0.40 -5 3 0 1.00 0.50 5 3 0 1.10 0.40 6 -3 0 87.09 3.40 6 -3 0 85.29 3.30 6 3 0 83.69 3.20 7 -3 0 32.40 2.20 7 -3 0 33.90 2.00 7 3 0 29.30 2.00 8 -3 0 223.48 7.80 -8 -3 0 247.08 7.70 -8 -3 0 231.78 7.80 -8 -3 0 234.18 7.80 -8 3 0 235.58 8.10 9 -3 0 5.90 1.30 -9 -3 0 7.70 1.20 -9 -3 0 7.60 1.40 -9 -3 0 4.90 1.40 -9 3 0 3.30 1.10 10 -3 0 163.38 5.90 -10 -3 0 169.78 5.90 -10 -3 0 166.98 6.60 -10 -3 0 167.28 5.90 -11 -3 0 440.56 14.20 11 -3 0 435.76 14.00 -11 -3 0 455.75 14.10 -11 -3 0 439.36 14.00 -11 3 0 444.76 14.20 -11 3 0 450.65 14.10 -12 -3 0 2.90 1.00 12 -3 0 2.80 1.20 -12 -3 0 0.10 0.70 -12 -3 0 1.40 0.80 -12 3 0 1.30 0.80 -12 3 0 -0.10 0.70 -13 -3 0 5.40 1.10 -13 -3 0 7.30 1.60 -13 3 0 7.20 1.30 -13 3 0 7.40 1.30 -14 -3 0 11.40 1.20 -14 3 0 10.50 1.20 -14 3 0 7.30 1.30 -15 -3 0 12.10 1.10 -15 3 0 13.70 1.10 -15 3 0 12.20 1.30 -16 -3 0 22.80 1.20 -16 3 0 25.90 1.30 0 4 0 601.54 18.20 1 -4 0 123.79 4.30 1 4 0 133.69 4.20 1 4 0 121.69 4.30 -1 4 0 128.49 4.20 2 -4 0 76.89 2.90 2 -4 0 71.79 3.00 -2 4 0 83.19 2.90 2 4 0 86.09 3.00 2 4 0 82.19 2.80 3 -4 0 373.36 12.00 3 -4 0 393.36 12.00 -3 4 0 389.26 11.90 4 -4 0 69.09 2.80 4 -4 0 66.99 2.80 4 4 0 68.49 2.60 -4 4 0 67.89 2.70 5 -4 0 502.45 15.90 5 -4 0 493.45 15.80 5 4 0 537.15 15.80 6 -4 0 0.50 0.80 6 -4 0 1.40 0.70 6 4 0 0.60 0.70 -7 -4 0 27.50 2.00 -7 -4 0 26.40 1.80 -7 -4 0 29.70 1.80 7 -4 0 25.60 1.90 8 -4 0 141.29 5.10 -8 -4 0 142.69 5.10 -8 -4 0 138.49 5.00 -8 -4 0 140.19 4.90 -8 4 0 124.99 5.00 9 -4 0 24.60 2.20 -9 -4 0 20.10 1.60 -9 -4 0 23.20 1.80 -9 -4 0 29.10 1.90 -9 4 0 24.60 2.00 -10 -4 0 181.38 6.40 -10 -4 0 181.28 6.40 -10 -4 0 183.58 6.30 -10 4 0 185.18 6.40 -11 -4 0 156.08 5.80 -11 -4 0 151.08 5.50 -11 -4 0 159.18 5.50 -11 4 0 150.18 5.60 -11 4 0 151.18 5.50 -12 -4 0 0.10 0.70 -12 -4 0 -0.10 0.70 -12 -4 0 0.60 0.70 -12 4 0 0.40 0.70 -12 4 0 0.70 0.90 -13 -4 0 1.10 1.10 -13 -4 0 0.20 0.80 -13 4 0 -0.50 0.60 -13 4 0 0.60 0.90 -14 -4 0 16.90 1.30 -14 -4 0 16.90 1.60 -14 4 0 14.70 1.50 -14 4 0 16.30 1.30 -15 -4 0 17.50 1.20 -15 4 0 18.70 1.20 -16 -4 0 5.70 0.80 -16 4 0 6.00 0.80 0 -5 0 -0.10 0.70 0 5 0 0.60 0.50 -1 -5 0 -0.10 0.60 2 -5 0 4.00 1.10 2 -5 0 3.80 1.00 -2 -5 0 4.20 0.90 -2 5 0 3.60 1.10 2 5 0 4.70 0.80 2 5 0 3.70 1.20 3 -5 0 55.59 2.50 -3 -5 0 56.79 2.60 3 5 0 58.59 2.40 3 5 0 63.49 3.20 4 -5 0 1056.59 32.60 4 -5 0 1079.99 32.80 4 5 0 1098.49 32.50 5 -5 0 74.59 3.20 5 -5 0 74.99 3.60 5 5 0 79.99 3.30 6 -5 0 15.20 1.40 -6 -5 0 16.30 1.40 -6 -5 0 15.00 1.50 -7 -5 0 65.29 2.80 7 -5 0 66.59 3.00 -7 -5 0 65.99 2.90 -7 -5 0 65.49 3.10 -8 -5 0 4.40 1.20 -8 -5 0 3.70 1.10 -8 -5 0 2.00 1.00 8 -5 0 3.20 1.00 -9 -5 0 42.50 2.30 9 -5 0 44.60 2.70 -9 -5 0 46.10 2.50 -9 -5 0 45.30 2.20 -10 -5 0 5.40 1.20 -10 -5 0 5.20 1.10 10 -5 0 4.20 1.30 -10 -5 0 5.30 1.10 -11 -5 0 4.60 1.00 -11 -5 0 6.30 1.40 -11 -5 0 4.50 1.20 -11 5 0 3.60 0.90 -12 -5 0 93.79 3.70 -12 -5 0 92.09 3.80 -12 -5 0 97.69 3.70 -12 5 0 98.19 3.90 -13 -5 0 25.00 1.60 -13 -5 0 25.10 1.70 -13 -5 0 24.20 1.40 -13 5 0 23.20 1.60 -14 -5 0 -0.40 0.60 -14 -5 0 0.50 0.50 -14 -5 0 0.70 0.70 -14 5 0 0.80 0.50 -15 -5 0 0.00 0.50 -15 5 0 0.10 0.40 0 -6 0 357.16 11.40 1 -6 0 1.40 0.70 -1 -6 0 1.90 0.80 1 6 0 2.90 0.70 2 -6 0 110.29 4.20 -2 -6 0 109.39 4.10 2 6 0 110.09 4.20 3 -6 0 258.37 9.00 -3 -6 0 260.07 8.50 3 6 0 265.17 8.70 4 -6 0 19.40 1.50 -4 -6 0 19.20 1.60 -4 -6 0 14.80 1.80 -4 -6 0 17.90 1.70 5 -6 0 0.50 0.70 -5 -6 0 -1.00 0.90 -5 -6 0 -0.20 0.80 5 -6 0 2.10 0.90 -6 -6 0 51.59 2.40 6 -6 0 51.39 2.40 -6 -6 0 49.30 3.00 6 -6 0 52.29 2.70 -6 -6 0 51.59 2.50 7 -6 0 53.89 2.80 -7 -6 0 52.79 2.50 -7 -6 0 48.20 2.80 -7 -6 0 55.89 2.60 -8 -6 0 30.20 1.90 -8 -6 0 29.10 1.80 -8 -6 0 31.60 2.30 8 -6 0 32.30 2.20 -9 -6 0 35.00 2.00 -9 -6 0 38.90 2.30 9 -6 0 35.70 2.40 -9 -6 0 33.10 2.10 -10 -6 0 76.09 3.30 -10 -6 0 77.79 3.40 -10 -6 0 73.29 3.70 10 -6 0 79.39 3.80 -11 -6 0 34.70 1.90 -11 -6 0 36.50 2.00 -11 -6 0 34.70 2.10 -11 6 0 36.40 2.10 -12 -6 0 15.60 1.50 -12 -6 0 13.20 1.30 -12 -6 0 14.30 1.20 -12 6 0 13.70 1.40 -13 -6 0 75.09 3.00 -13 -6 0 78.09 2.90 -13 -6 0 69.79 2.80 -13 6 0 71.09 3.00 -14 -6 0 7.20 1.30 -14 -6 0 4.50 0.70 -14 -6 0 5.80 1.10 -14 6 0 5.30 0.90 -15 6 0 1.30 0.50 0 -7 0 -1.60 1.00 0 -7 0 -0.50 0.70 -1 -7 0 161.88 5.50 1 -7 0 156.58 5.60 1 -7 0 148.29 5.50 -1 -7 0 145.39 5.40 -2 -7 0 13.90 1.90 -2 -7 0 13.30 1.60 2 -7 0 11.00 1.40 -2 -7 0 15.00 1.50 2 -7 0 15.00 1.90 -3 -7 0 202.48 6.50 3 -7 0 176.58 6.50 -3 -7 0 192.08 6.60 -3 -7 0 206.18 6.70 3 -7 0 178.98 6.70 3 -7 0 190.18 6.80 4 -7 0 7.30 1.70 4 -7 0 7.20 1.60 4 -7 0 9.10 2.10 -4 -7 0 10.40 1.30 -4 -7 0 9.80 1.80 -4 -7 0 8.00 1.50 5 -7 0 121.39 4.90 -5 -7 0 124.49 4.60 5 -7 0 122.49 4.60 -5 -7 0 128.89 4.60 6 -7 0 70.09 2.90 -6 -7 0 70.29 3.70 6 -7 0 67.29 3.70 -6 -7 0 57.19 3.90 -7 -7 0 21.40 1.70 7 -7 0 25.70 2.00 -7 -7 0 23.10 1.60 8 -7 0 46.90 2.70 -8 -7 0 41.00 2.20 -8 -7 0 45.30 2.40 -8 -7 0 45.30 2.70 -9 -7 0 15.90 1.40 -9 -7 0 16.90 1.90 9 -7 0 15.50 1.90 -9 -7 0 16.10 1.70 -10 -7 0 233.58 7.60 10 -7 0 207.38 7.90 -10 -7 0 233.38 7.70 -10 -7 0 231.08 7.70 -11 -7 0 17.90 1.60 -11 -7 0 17.60 1.50 -11 -7 0 23.20 1.80 -11 7 0 19.50 1.60 -12 -7 0 32.20 1.70 -12 -7 0 33.50 2.00 -12 -7 0 33.10 1.90 -12 7 0 31.80 1.80 -13 -7 0 4.10 0.70 -13 -7 0 4.80 1.20 -13 -7 0 3.60 0.80 -13 7 0 3.70 0.80 -14 -7 0 6.40 0.80 -14 7 0 7.10 0.80 0 -8 0 185.28 6.60 0 -8 0 180.48 6.30 1 -8 0 117.29 4.70 -1 -8 0 125.69 4.70 -1 -8 0 116.09 4.40 1 -8 0 117.19 4.50 2 -8 0 159.28 5.90 -2 -8 0 152.68 5.50 2 -8 0 155.28 5.50 -2 -8 0 147.49 5.50 -2 -8 0 151.78 5.60 -3 -8 0 22.30 1.90 -3 -8 0 26.00 2.00 3 -8 0 25.00 1.90 -3 -8 0 21.30 1.70 3 -8 0 18.00 2.00 4 -8 0 11.60 1.70 4 -8 0 13.60 1.60 4 -8 0 9.60 2.10 -4 -8 0 8.50 2.30 -4 -8 0 13.60 1.40 -4 -8 0 12.40 1.90 -5 -8 0 35.60 2.10 5 -8 0 37.60 2.40 -5 -8 0 34.80 2.00 -6 -8 0 29.20 1.90 -6 -8 0 31.50 1.90 6 -8 0 32.90 2.60 7 -8 0 462.95 15.50 -7 -8 0 484.65 15.00 -7 -8 0 485.35 15.10 -8 -8 0 21.50 1.60 -8 -8 0 20.30 1.80 8 -8 0 18.20 1.90 -9 -8 0 37.90 2.00 9 -8 0 32.50 2.40 -9 -8 0 36.40 2.10 -10 -8 0 29.00 1.60 10 -8 0 28.90 2.30 -10 -8 0 30.30 1.80 -10 8 0 29.60 1.80 -11 -8 0 21.80 1.40 -11 -8 0 23.60 1.30 -11 8 0 21.40 1.50 -12 -8 0 9.40 1.00 -12 -8 0 11.40 1.00 -12 8 0 11.00 1.00 -13 -8 0 8.10 0.80 -13 -8 0 7.00 0.70 -13 8 0 6.40 0.80 0 -9 0 -1.20 0.80 0 -9 0 -0.70 1.00 1 -9 0 145.69 5.60 -1 -9 0 148.09 5.50 -1 -9 0 140.09 5.20 1 -9 0 139.29 5.20 -2 -9 0 161.78 5.90 -2 -9 0 150.68 5.60 2 -9 0 155.78 5.60 2 -9 0 159.68 6.00 -2 -9 0 153.88 5.50 3 -9 0 45.00 2.60 -3 -9 0 46.80 2.70 -3 -9 0 50.29 2.40 -3 -9 0 49.30 2.60 3 -9 0 46.90 2.80 -4 -9 0 -0.50 0.80 -4 -9 0 0.60 0.70 -5 -9 0 114.39 4.30 5 -9 0 107.39 4.70 -5 -9 0 112.29 4.20 6 -9 0 157.18 6.30 -6 -9 0 172.08 5.80 -6 -9 0 168.78 5.90 -7 -9 0 285.17 9.40 -7 -9 0 301.77 9.50 7 -9 0 274.17 9.80 -8 -9 0 200.58 6.60 -8 -9 0 200.88 6.80 8 -9 0 186.78 7.00 -9 -9 0 81.99 3.30 -9 -9 0 81.29 3.20 9 -9 0 85.89 3.70 -9 9 0 81.79 3.30 -10 -9 0 65.09 2.70 -10 -9 0 64.59 2.60 10 -9 0 65.59 3.20 -10 9 0 63.99 2.70 -11 -9 0 27.10 1.40 -11 -9 0 26.30 1.40 -11 9 0 27.80 1.50 -12 -9 0 0.00 0.40 -12 -9 0 0.10 0.40 -12 9 0 0.20 0.50 0 -10 0 104.39 3.90 0 -10 0 96.39 4.30 -1 -10 0 356.66 12.10 -1 -10 0 381.76 11.80 1 -10 0 382.96 11.80 1 -10 0 351.36 12.20 -2 -10 0 685.63 21.30 -2 -10 0 681.33 20.90 2 -10 0 649.14 21.40 2 -10 0 705.13 20.90 3 -10 0 4.10 1.10 -3 -10 0 3.20 0.80 -3 -10 0 6.80 1.60 -4 -10 0 265.57 8.50 -4 -10 0 273.17 8.60 4 -10 0 240.28 9.80 -5 -10 0 9.10 1.20 5 -10 0 8.50 1.50 -5 -10 0 6.50 1.30 6 -10 0 0.00 0.80 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32.50 -1 4 4 993.50 32.30 0 -4 -4 335.07 10.80 0 -4 4 351.46 10.80 0 4 4 348.97 10.80 0 4 -4 340.97 10.60 0 4 4 353.46 11.00 1 -4 4 3.20 0.80 1 -4 4 2.60 0.80 1 4 4 1.60 0.40 -1 4 -4 2.70 0.80 1 4 4 1.60 0.70 2 -4 4 1.00 0.50 2 -4 4 0.00 0.50 2 4 4 0.10 0.40 -2 4 -4 0.80 0.50 3 -4 4 2.50 0.70 3 -4 4 2.80 0.90 -3 4 -4 2.80 0.70 3 4 4 3.00 0.80 3 4 4 1.70 0.60 4 -4 4 59.39 2.60 4 -4 4 58.69 2.90 4 4 4 57.79 2.50 4 4 4 59.49 2.90 -5 -4 -4 145.79 5.20 -5 -4 -4 144.89 5.20 5 -4 4 152.08 5.30 5 -4 4 151.68 5.10 5 4 4 146.29 5.10 6 -4 4 27.00 1.80 -6 -4 -4 25.10 2.20 -6 -4 -4 31.10 1.90 6 -4 4 29.60 1.70 -6 -4 -4 27.90 1.80 7 -4 4 120.99 4.50 -7 -4 -4 126.29 4.60 -7 -4 -4 116.29 4.60 7 -4 4 128.29 4.70 -7 -4 -4 125.59 4.50 8 -4 4 0.40 0.70 -8 -4 -4 0.00 0.90 -8 -4 -4 1.70 0.90 8 -4 4 2.80 0.90 -8 -4 -4 1.00 0.90 -8 4 -4 1.50 0.70 9 -4 4 19.80 2.00 -9 -4 -4 21.30 1.80 -9 -4 -4 21.90 1.70 -9 -4 -4 19.80 1.60 -9 4 -4 19.10 1.60 -10 -4 -4 62.99 2.90 -10 -4 -4 61.89 2.90 -10 -4 -4 63.69 2.80 -10 4 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55.39 2.80 -3 -5 -4 58.19 2.60 -3 -5 -4 62.29 2.70 3 -5 4 55.59 2.50 3 -5 4 58.09 3.10 3 -5 4 58.69 2.60 4 -5 4 21.20 1.60 -4 -5 -4 23.40 1.70 4 -5 4 22.30 1.80 4 -5 4 22.20 1.50 -4 -5 -4 20.60 1.70 4 5 4 21.80 1.60 5 -5 4 79.89 3.30 -5 -5 -4 74.89 3.10 -5 -5 -4 75.99 3.20 5 -5 4 79.69 3.10 5 5 4 74.69 3.20 6 -5 4 78.19 3.10 -6 -5 -4 72.79 3.10 -6 -5 -4 79.49 3.30 6 -5 4 72.79 3.30 -7 -5 -4 54.49 2.60 -7 -5 -4 51.19 2.90 7 -5 4 55.99 2.80 7 -5 4 54.99 2.50 -7 -5 -4 53.79 2.60 8 -5 4 331.87 11.20 -8 -5 -4 338.17 11.30 -8 -5 -4 351.56 11.20 -8 -5 -4 356.16 11.30 8 -5 4 370.66 11.60 -8 5 -4 352.56 11.20 -9 -5 -4 4.90 1.20 -9 -5 -4 6.00 1.20 9 -5 4 6.00 1.70 -9 -5 -4 4.80 1.10 -9 5 -4 2.80 0.80 10 -5 4 3.30 1.40 -10 -5 -4 1.20 0.90 -10 -5 -4 2.30 0.70 -10 -5 -4 1.90 0.80 -10 5 -4 4.30 1.20 -11 -5 -4 0.70 0.60 -11 -5 -4 1.30 0.80 -11 -5 -4 -0.40 0.70 -11 5 -4 1.20 0.70 -12 -5 -4 -0.40 0.60 -12 -5 -4 0.70 0.70 -12 -5 -4 -1.10 0.80 -12 5 -4 0.30 0.50 -12 5 -4 1.60 0.70 -13 -5 -4 -1.30 0.70 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2.80 5 -6 4 59.99 3.00 -5 -6 -4 63.99 2.80 5 6 4 63.89 2.90 6 -6 4 13.50 1.30 -6 -6 -4 13.40 1.40 6 -6 4 11.30 1.50 -6 -6 -4 15.10 1.50 7 -6 4 279.47 9.10 7 -6 4 294.07 9.60 -7 -6 -4 276.47 9.30 -7 -6 -4 270.57 9.10 -7 6 -4 274.87 9.00 8 -6 4 3.40 1.00 -8 -6 -4 6.60 1.20 -8 6 -4 2.80 0.90 9 -6 4 71.29 3.40 -9 -6 -4 75.89 3.20 -9 -6 -4 73.99 3.10 -9 -6 -4 74.69 3.30 -9 6 -4 77.39 3.10 -10 -6 -4 8.00 1.20 10 -6 4 11.30 2.10 -10 -6 -4 11.30 1.70 -10 -6 -4 10.50 1.10 -10 6 -4 9.70 1.40 -11 -6 -4 0.60 1.00 -11 -6 -4 0.70 0.60 -11 -6 -4 0.30 0.50 -11 6 -4 -0.50 0.80 -11 6 -4 0.10 0.60 -12 -6 -4 18.00 1.10 -12 -6 -4 20.60 1.50 -12 6 -4 16.80 1.20 -13 6 -4 3.20 0.70 -15 -7 4 9.00 0.80 -15 -7 4 8.60 0.90 -15 7 4 11.10 0.90 -14 -7 4 10.30 1.00 -14 -7 4 10.20 0.90 -14 7 4 9.20 1.10 -13 -7 4 9.80 1.20 -13 -7 4 12.20 1.10 13 -7 -4 11.50 1.30 -13 7 4 9.70 1.10 -12 -7 4 22.30 1.60 -12 -7 4 20.20 1.50 12 -7 -4 20.30 1.60 -12 -7 4 22.90 1.40 -12 7 4 19.00 1.60 11 -7 -4 35.20 2.10 -11 -7 4 33.90 2.10 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50.09 2.60 -5 -2 9 50.39 2.50 -5 2 9 53.69 2.40 -4 -2 9 32.50 1.80 -4 -2 9 33.20 2.70 4 -2 -9 30.30 1.90 -4 2 9 32.60 1.80 3 -2 -9 34.30 2.00 -3 -2 9 36.40 1.80 2 -2 -9 198.28 7.00 -2 -2 9 187.08 6.30 -2 2 9 185.88 6.40 -1 -2 9 56.39 2.40 1 -2 -9 51.29 2.50 -1 -2 9 53.69 2.50 -1 2 9 57.89 2.40 0 -2 9 18.40 1.30 0 -2 -9 15.40 1.60 0 -2 9 16.10 1.40 0 2 9 17.50 1.30 1 -2 9 0.00 1.00 1 -2 9 1.90 0.80 1 -2 9 0.60 0.50 -1 -2 -9 1.90 1.00 1 2 9 1.00 0.50 2 -2 9 131.59 4.70 2 -2 9 134.79 4.60 -2 -2 -9 126.39 4.70 2 -2 9 122.49 4.60 2 2 9 128.59 4.70 3 -2 9 9.60 1.20 -3 -2 -9 8.20 1.60 -3 -2 -9 10.30 1.70 3 -2 9 9.30 1.30 3 -2 9 9.70 1.50 3 2 9 9.50 1.10 -4 -2 -9 4.20 1.20 -4 -2 -9 3.20 0.90 4 -2 9 1.90 0.70 4 -2 9 1.70 0.90 4 2 9 1.90 0.70 -5 -2 -9 229.18 7.70 5 -2 9 234.48 7.70 5 -2 9 241.18 8.00 5 2 9 229.98 7.90 6 -2 9 2.40 1.00 -6 -2 -9 5.00 1.30 6 2 9 6.20 1.50 -7 -2 -9 28.30 1.80 7 -2 9 29.40 2.00 -7 2 -9 26.30 1.70 7 2 9 26.50 2.00 -8 -2 -9 19.60 1.50 8 -2 9 17.50 1.80 -8 2 -9 16.40 1.40 -9 -2 -9 33.90 1.90 -9 2 -9 36.50 1.80 -10 -2 -9 10.90 1.10 -10 2 -9 11.00 1.00 -11 -2 -9 27.30 1.40 -11 2 -9 27.40 1.40 17 -3 -9 0.30 0.40 -17 -3 9 0.00 0.60 -17 -3 9 0.80 0.50 17 3 -9 -0.30 0.40 -17 3 9 0.20 0.40 -16 -3 9 56.09 2.30 16 -3 -9 54.79 2.30 -16 -3 9 55.69 2.30 16 3 -9 55.99 2.20 -16 3 9 50.99 2.30 -15 -3 9 7.60 1.10 15 -3 -9 6.60 1.10 -15 -3 9 6.10 1.10 -15 -3 9 7.60 1.10 15 3 -9 8.50 1.00 -15 3 9 9.00 1.10 14 -3 -9 2.20 0.70 -14 -3 9 4.60 1.10 -14 -3 9 3.50 1.00 -14 -3 9 4.90 1.10 -14 3 9 4.40 1.20 13 -3 -9 84.39 3.70 -13 -3 9 95.49 3.70 -13 -3 9 89.99 3.70 13 -3 -9 91.49 3.60 -13 -3 9 86.59 3.70 -13 3 9 88.89 3.80 12 -3 -9 50.39 2.60 -12 -3 9 45.00 2.50 -12 -3 9 49.90 2.60 -12 -3 9 47.80 2.50 12 -3 -9 50.09 2.50 -12 3 9 45.40 2.60 11 -3 -9 32.40 2.00 -11 -3 9 29.90 2.30 -11 -3 9 30.40 2.00 11 -3 -9 31.30 2.00 -11 -3 9 31.00 2.10 -11 3 9 32.90 2.20 10 -3 -9 222.18 7.50 -10 -3 9 219.28 7.50 -10 -3 9 214.78 7.50 -10 -3 9 211.78 7.50 -10 3 9 214.68 7.50 -9 -3 9 9.20 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10.20 2 -3 9 20.40 1.40 2 -3 9 19.90 1.50 -2 -3 -9 19.10 1.70 2 -3 9 20.60 1.60 2 3 9 16.30 1.40 3 -3 9 52.19 2.40 3 -3 9 55.59 2.60 3 -3 9 54.19 2.50 -3 -3 -9 54.39 2.60 3 3 9 51.99 2.50 -4 -3 -9 70.39 3.20 4 -3 9 71.89 3.00 4 -3 9 72.19 3.20 4 3 9 74.89 3.10 -5 -3 -9 151.98 5.50 5 -3 9 147.29 5.30 -5 -3 -9 152.88 5.40 5 -3 9 155.18 5.60 5 3 9 153.18 5.50 6 -3 9 1.80 0.80 -6 -3 -9 -0.40 1.00 -6 -3 -9 3.70 1.00 6 -3 9 1.40 0.80 6 3 9 2.00 0.90 -7 -3 -9 49.10 2.40 7 -3 9 45.90 2.50 -7 3 -9 46.20 2.30 7 3 9 45.90 2.60 8 -3 9 -0.20 0.90 -8 -3 -9 0.70 0.80 -8 3 -9 1.30 0.60 -9 -3 -9 6.00 1.20 9 -3 9 5.60 1.40 -9 3 -9 5.70 1.50 -9 3 -9 4.50 0.90 -10 -3 -9 49.80 2.20 -10 3 -9 51.49 2.10 -11 3 -9 78.49 2.90 17 -4 -9 34.40 1.40 17 4 -9 29.50 1.40 -17 4 9 32.80 1.40 16 -4 -9 0.70 0.50 -16 -4 9 0.70 0.50 -16 -4 9 0.40 0.60 16 4 -9 1.40 0.50 -16 4 9 0.90 0.50 -15 -4 9 73.69 2.90 15 -4 -9 74.39 3.00 -15 -4 9 71.49 2.90 -15 -4 9 75.89 2.90 -15 4 9 73.79 3.00 15 4 -9 71.39 2.80 -14 -4 9 6.80 1.10 14 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4 -4 9 928.01 29.00 4 -4 9 967.10 29.40 -4 -4 -9 952.90 29.20 4 4 9 981.10 29.20 5 -4 9 118.99 4.70 5 -4 9 120.09 4.40 -5 -4 -9 127.29 4.50 5 4 9 108.69 5.30 6 -4 9 223.38 8.00 6 -4 9 241.28 7.60 -6 -4 -9 236.78 7.70 6 4 9 218.88 7.70 7 -4 9 160.68 6.10 -7 -4 -9 173.08 5.90 -7 4 -9 174.28 5.90 8 -4 9 20.10 1.80 -8 4 -9 20.20 1.40 9 -4 9 2.00 1.30 -9 4 -9 1.10 0.50 -10 4 -9 5.20 0.70 -11 4 -9 4.30 0.70 -16 -5 9 3.90 0.70 16 -5 -9 5.50 0.70 -16 5 9 4.50 0.90 16 5 -9 3.70 0.80 -15 -5 9 30.50 1.60 15 -5 -9 34.30 1.80 -15 -5 9 30.80 1.60 -15 -5 9 32.20 1.70 15 5 -9 31.90 1.50 -15 5 9 33.20 1.70 -14 -5 9 5.80 1.10 -14 -5 9 4.00 1.00 -14 -5 9 5.10 1.00 -14 5 9 3.70 1.10 -13 -5 9 12.70 1.40 -13 -5 9 12.00 1.20 -13 -5 9 9.00 1.30 13 -5 -9 13.30 1.30 -13 5 9 13.80 1.50 -12 -5 9 174.28 6.10 -12 -5 9 161.78 6.00 -12 -5 9 171.88 6.00 12 -5 -9 167.08 6.10 -12 5 9 172.58 6.00 11 -5 -9 155.78 5.90 -11 -5 9 161.38 5.70 -11 -5 9 155.68 5.90 -11 -5 9 154.78 5.70 -11 5 9 156.88 5.70 -10 -5 9 215.88 7.40 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10 4.90 1.40 10 -2 -10 81.59 3.40 -10 -2 10 76.49 3.40 -10 -2 10 71.79 3.30 -10 -2 10 78.79 3.40 -10 2 10 75.79 3.40 -9 -2 10 36.00 2.20 9 -2 -10 28.70 3.30 -9 -2 10 33.20 2.90 -9 -2 10 37.00 2.20 -9 2 10 35.50 2.30 8 -2 -10 6.70 1.50 -8 -2 10 12.10 1.50 -8 -2 10 9.90 1.40 -8 -2 10 9.60 1.50 -8 2 10 8.90 1.80 -7 -2 10 67.19 2.90 -7 -2 10 67.49 3.00 7 -2 -10 60.99 3.00 -7 -2 10 69.39 2.90 -7 2 10 63.89 2.90 -7 2 10 59.89 3.20 -6 -2 10 9.10 1.50 -6 -2 10 6.70 1.50 -6 -2 10 7.30 1.40 6 -2 -10 7.60 1.80 -6 2 10 10.20 1.40 -6 2 10 7.20 1.60 -5 -2 10 60.39 2.80 -5 -2 10 61.09 2.90 -5 -2 10 65.09 2.90 -5 -2 10 60.59 3.00 5 -2 -10 67.49 2.80 5 -2 -10 55.69 3.20 -5 2 10 64.99 2.70 4 -2 -10 12.70 1.40 -4 -2 10 12.10 1.50 -4 -2 10 12.50 1.50 -4 -2 10 14.40 1.30 -4 2 10 11.10 1.20 -3 -2 10 64.19 2.70 -3 -2 10 62.39 2.80 3 -2 -10 61.29 2.80 -3 -2 10 61.99 2.80 -3 2 10 67.49 2.80 2 -2 -10 10.70 1.40 -2 -2 10 9.70 1.40 -2 -2 10 9.60 1.10 -2 -2 10 9.70 1.50 -2 2 10 9.80 1.10 1 -2 -10 129.99 4.60 -1 -2 10 119.69 4.60 -1 -2 10 126.09 4.60 -1 -2 10 128.09 4.60 -1 2 10 130.29 4.60 0 -2 10 11.90 1.30 0 -2 10 13.80 1.60 0 -2 -10 13.20 1.50 0 -2 10 11.20 1.10 0 2 10 10.20 1.10 -1 -2 -10 31.80 2.00 1 -2 10 30.20 1.90 1 -2 10 32.00 2.10 1 -2 10 29.70 1.80 1 2 10 30.30 1.80 2 -2 10 89.79 3.50 2 -2 10 90.59 3.60 -2 -2 -10 90.89 3.70 2 -2 10 89.49 3.60 2 2 10 91.89 3.60 3 -2 10 174.18 6.20 -3 -2 -10 168.38 6.10 3 -2 10 170.48 6.00 -3 -2 -10 173.88 6.00 3 2 10 181.78 6.20 4 -2 10 152.88 5.60 4 -2 10 151.38 5.40 -4 -2 -10 150.68 5.60 -4 -2 -10 157.08 5.40 4 2 10 156.88 5.60 5 -2 10 -0.50 0.90 5 -2 10 0.50 0.70 5 2 10 0.70 0.80 6 -2 10 41.80 2.30 -6 -2 -10 40.30 2.20 6 2 10 38.30 2.20 -6 2 -10 41.70 2.10 -7 -2 -10 162.68 5.80 7 -2 10 160.38 5.90 7 2 10 163.28 5.90 -7 2 -10 168.98 5.70 -8 -2 -10 141.59 4.90 8 -2 10 140.19 5.20 -8 2 -10 135.89 4.90 -9 -2 -10 11.00 1.10 -9 2 -10 9.90 1.00 -10 -2 -10 1.90 0.60 -10 2 -10 0.80 0.40 -11 2 -10 19.60 1.00 -17 -3 10 24.50 1.30 -17 -3 10 27.80 1.30 17 -3 -10 28.90 1.30 -17 3 10 26.40 1.30 17 3 -10 29.50 1.30 -16 -3 10 45.20 2.00 16 -3 -10 47.00 2.00 -16 -3 10 43.70 1.90 16 3 -10 46.30 1.90 -16 3 10 47.70 2.10 -15 -3 10 3.90 1.00 -15 -3 10 2.10 0.70 15 -3 -10 2.80 0.90 -15 3 10 3.90 1.00 15 3 -10 4.30 0.90 -14 -3 10 21.50 1.60 14 -3 -10 21.80 1.60 -14 -3 10 23.00 1.60 -14 -3 10 22.20 1.60 -14 3 10 22.30 1.70 14 3 -10 23.00 1.60 13 -3 -10 7.50 1.20 13 -3 -10 7.40 1.40 -13 -3 10 8.00 1.20 -13 -3 10 10.10 1.20 -13 -3 10 6.70 1.30 -13 3 10 6.40 1.40 -12 -3 10 117.39 4.70 12 -3 -10 122.19 4.50 -12 -3 10 118.39 4.70 12 -3 -10 125.19 4.70 -12 -3 10 120.09 4.70 -12 3 10 123.09 4.70 11 -3 -10 0.80 0.80 11 -3 -10 0.30 0.80 -11 -3 10 2.20 0.80 -11 -3 10 1.60 0.90 -11 -3 10 1.50 0.80 -11 3 10 1.10 0.90 10 -3 -10 0.50 0.80 10 -3 -10 -0.40 0.70 -10 -3 10 0.10 0.80 -10 -3 10 0.90 0.80 -10 -3 10 -0.20 0.70 -10 3 10 -1.00 0.90 -9 -3 10 9.90 1.40 -9 -3 10 10.20 1.40 9 -3 -10 9.10 1.50 9 -3 -10 7.70 1.40 -9 -3 10 13.20 1.50 -9 3 10 8.70 1.80 -8 -3 10 198.38 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0.70 -5 -4 10 2.40 1.10 5 -4 -10 0.30 0.70 5 -4 -10 0.00 0.90 -5 -4 10 1.20 0.80 -5 4 10 1.10 0.80 4 -4 -10 66.79 3.10 -4 -4 10 64.49 3.00 4 -4 -10 67.99 2.90 -4 -4 10 67.29 3.00 -4 -4 10 65.99 2.90 -4 4 10 70.79 3.00 -3 -4 10 17.90 1.50 -3 -4 10 20.10 1.60 3 -4 -10 19.30 1.50 -3 -4 10 20.00 1.60 3 -4 -10 19.30 1.90 -3 4 10 18.90 1.50 -2 -4 10 8.60 1.30 2 -4 -10 8.10 1.30 -2 -4 10 9.40 1.30 -2 -4 10 9.60 1.20 2 -4 -10 11.10 1.80 -2 4 10 7.80 1.20 1 -4 -10 249.18 8.50 -1 -4 10 256.07 8.50 -1 -4 10 248.08 8.40 -1 -4 10 260.37 8.40 1 -4 -10 255.17 8.40 -1 4 10 260.87 8.60 0 -4 10 54.29 2.50 0 -4 -10 48.00 2.80 0 -4 -10 53.59 2.50 0 -4 10 54.29 2.60 0 -4 10 48.70 2.60 0 4 10 51.49 2.50 -1 -4 -10 41.70 2.30 1 -4 10 47.00 2.30 1 -4 10 46.20 2.40 1 -4 10 43.00 2.20 1 4 10 45.90 2.30 2 -4 10 16.80 1.40 2 -4 10 15.50 1.40 2 -4 10 15.40 1.50 -2 -4 -10 15.70 1.50 2 4 10 15.80 1.40 -3 -4 -10 29.00 1.90 3 -4 10 31.30 2.00 3 -4 10 29.20 1.80 3 -4 10 29.90 1.80 3 4 10 34.90 2.00 4 -4 10 219.78 7.30 4 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-18 22.80 1.20 11 1 -18 25.20 1.20 10 -1 -18 -0.40 0.40 10 1 -18 0.40 0.50 9 -1 -18 0.30 0.50 9 1 -18 0.20 0.50 8 -1 -18 3.60 0.80 8 1 -18 2.10 0.70 7 -1 -18 1.10 0.50 7 1 -18 0.60 0.70 6 -1 -18 29.50 1.50 5 -1 -18 41.20 2.10 4 -1 -18 27.20 1.60 -3 1 18 94.09 3.80 11 -2 -18 104.59 3.40 11 2 -18 96.19 3.30 10 -2 -18 120.09 4.10 10 2 -18 128.79 4.10 9 -2 -18 29.90 1.40 9 2 -18 28.00 1.40 8 -2 -18 7.80 0.80 8 2 -18 7.90 1.20 7 -2 -18 9.30 0.90 6 -2 -18 27.20 1.40 5 -2 -18 1.50 0.60 4 -2 -18 1.40 0.60 10 -3 -18 0.00 0.40 -9 -3 18 65.59 2.40 9 -3 -18 66.89 2.50 8 -3 -18 -0.20 0.40 -8 -3 18 0.40 0.60 -7 -3 18 44.10 1.90 7 -3 -18 49.40 2.00 -7 -3 18 45.00 1.90 6 -3 -18 4.00 0.80 5 -3 -18 1.80 0.70 4 -3 -18 23.60 1.30 3 -3 -18 24.90 1.40 -9 -4 18 13.20 1.10 9 -4 -18 16.40 0.90 -8 -4 18 4.50 0.80 8 -4 -18 4.00 0.70 -8 -4 18 6.90 1.00 -7 -4 18 1.10 0.60 -7 -4 18 2.10 0.60 7 -4 -18 0.30 0.40 6 -4 -18 -0.30 0.40 -6 -4 18 -0.10 0.80 5 -4 -18 2.50 0.70 4 -4 -18 3.40 0.70 3 -4 -18 1.30 0.60 7 -5 -18 0.20 0.40 6 -5 -18 0.40 0.40 5 -5 -18 -0.10 0.40 4 -5 -18 7.00 0.80 9 -1 -19 0.50 0.50 8 -1 -19 1.20 0.50 7 -1 -19 -0.60 0.60 8 -2 -19 50.09 1.90 7 -2 -19 14.70 1.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95818 _shelx_res_file ; TITL SKM263_0m_a.res in P2(1)/c SKM263_0m_a.res created by SHELXL-2018/1 at 15:16:07 on 19-Oct-2018 REM Old TITL SKM263_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.209, Rweak 0.006, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C24 F N6 O3 CELL 1.54178 14.4316 10.8518 15.5940 90.000 109.941 90.000 ZERR 1.000 0.0003 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H F N O S UNIT 96 94 4 16 17 4 TEMP -123 SIZE 0.11 0.137 0.147 L.S. 5 BOND $H LIST 5 FMAP 2 PLAN 5 ACTA 138 CONF EQIV $1 -x+1, y+1/2, -z+1/2 HTAB N4 N1_$1 EQIV $2 x, -y+3/2, z+1/2 HTAB C1 O5_$2 EQIV $3 -x+1, -y+2, -z+1 HTAB C7 O4_$3 EQIV $4 -x+2, -y+1, -z+1 HTAB C13 F1_$2 HTAB C16 N1_$1 EQIV $5 -x+1, -y+1, -z+1 EQIV $6 -x+1, y-1/2, -z+1/2 HTAB C16 O5_$6 HTAB C24 O1_$5 EQIV $7 x-1, y+1, z HTAB C24 O1_$7 HTAB O5 F1 EQIV $8 x, -y+3/2, z-1/2 HTAB O5 O3_$8 MPLA C5 > C10 MPLA 5 N1 N2 C2 C3 C4 C1 MPLA C18 > C23 MPLA C4 N2 C15 C16 S1 MPLA 5 N1 N2 C2 C3 C4 C1 WGHT 0.038900 1.163700 EXTI 0.002293 FVAR 0.41322 S1 6 0.457090 0.298462 0.225683 11.00000 0.01757 0.02598 = 0.03121 -0.00720 0.00266 0.00125 F1 3 0.819514 0.850953 0.244335 11.00000 0.10611 0.02628 = 0.11911 -0.00549 0.08884 -0.01711 O1 5 0.935918 0.243789 0.478030 11.00000 0.02139 0.03448 = 0.04756 -0.00548 0.00381 0.00928 O2 5 0.884387 0.416703 0.526844 11.00000 0.01772 0.03131 = 0.03257 -0.00566 0.00020 0.00262 O3 5 0.557057 0.718120 0.545500 11.00000 0.02706 0.03361 = 0.02739 -0.00388 0.00395 0.00383 O4 5 0.174202 1.046057 0.461655 11.00000 0.03705 0.04047 = 0.04001 -0.00511 0.01367 0.01747 N1 4 0.644449 0.227081 0.274154 11.00000 0.01976 0.01941 = 0.02571 -0.00127 0.00637 0.00096 N2 4 0.605602 0.398686 0.349176 11.00000 0.01511 0.01862 = 0.02459 -0.00133 0.00459 0.00115 N3 4 0.545603 0.556537 0.412658 11.00000 0.01744 0.02023 = 0.02462 0.00115 0.00782 0.00279 N4 4 0.465118 0.627372 0.411536 11.00000 0.01791 0.02164 = 0.02312 0.00055 0.00693 0.00445 H4 2 0.418163 0.641850 0.358650 11.00000 0.03157 C1 1 0.708734 0.432839 0.400346 11.00000 0.01511 0.02110 = 0.02559 -0.00278 0.00421 0.00006 H1 2 0.712209 0.451207 0.463363 11.00000 0.02236 C2 1 0.773245 0.322645 0.399181 11.00000 0.01695 0.02083 = 0.02837 0.00053 0.00622 0.00190 C3 1 0.741712 0.232331 0.335744 11.00000 0.01904 0.02049 = 0.02763 0.00234 0.00791 0.00157 C4 1 0.582869 0.305966 0.287311 11.00000 0.02057 0.01809 = 0.02298 0.00054 0.00673 -0.00014 C5 1 0.736844 0.547076 0.358074 11.00000 0.01465 0.01987 = 0.03482 -0.00205 0.00773 0.00122 C6 1 0.768695 0.653314 0.409737 11.00000 0.02074 0.02366 = 0.03991 -0.00567 0.00658 0.00067 H6 2 0.769578 0.654501 0.474393 11.00000 0.03496 C7 1 0.797561 0.756201 0.371831 11.00000 0.02700 0.02041 = 0.06405 -0.00925 0.01787 -0.00396 H7 2 0.822255 0.828853 0.409191 11.00000 0.04814 C8 1 0.791486 0.750328 0.282093 11.00000 0.04389 0.02044 = 0.07438 0.00006 0.04061 -0.00316 C9 1 0.757929 0.648623 0.227927 11.00000 0.05819 0.02704 = 0.05680 -0.00135 0.04024 -0.00182 H9 2 0.752554 0.651054 0.162868 11.00000 0.04964 C10 1 0.731340 0.545904 0.267298 11.00000 0.03729 0.02274 = 0.04033 -0.00507 0.02119 -0.00355 H10 2 0.706735 0.474479 0.230447 11.00000 0.03810 C11 1 0.871860 0.320070 0.469241 11.00000 0.01909 0.02379 = 0.03122 -0.00045 0.00638 0.00154 C12 1 0.979959 0.425613 0.598554 11.00000 0.01766 0.04312 = 0.03154 -0.00313 -0.00051 0.00040 H12A 2 0.987789 0.352982 0.640387 11.00000 0.04456 H12B 2 1.031606 0.421599 0.570305 11.00000 0.03411 H12C 2 0.964190 0.618278 0.601394 11.00000 0.05225 C13 1 0.981329 0.545414 0.646682 11.00000 0.02841 0.05602 = 0.03480 -0.01402 0.00529 -0.00247 H13A 2 1.049082 0.556587 0.692851 11.00000 0.05490 H13B 2 0.932900 0.545270 0.677609 11.00000 0.06040 C14 1 0.803545 0.126585 0.324058 11.00000 0.02393 0.02521 = 0.03562 -0.00367 0.00833 0.00504 H14A 2 0.864911 0.155188 0.318590 11.00000 0.05157 H14B 2 0.824002 0.073906 0.376410 11.00000 0.05366 H14C 2 0.766324 0.079202 0.269630 11.00000 0.04578 C15 1 0.527131 0.470983 0.353139 11.00000 0.01709 0.01863 = 0.02457 0.00282 0.00678 0.00108 C16 1 0.430992 0.432081 0.283436 11.00000 0.01874 0.02544 = 0.03028 -0.00481 0.00376 0.00195 H16A 2 0.403186 0.497385 0.238914 11.00000 0.03967 H16B 2 0.383946 0.409933 0.314141 11.00000 0.04251 C17 1 0.480234 0.711617 0.480387 11.00000 0.02259 0.02173 = 0.02342 0.00153 0.00899 0.00069 C18 1 0.394695 0.794306 0.471523 11.00000 0.02464 0.02351 = 0.02338 0.00024 0.01133 0.00231 C19 1 0.413590 0.902782 0.523287 11.00000 0.02869 0.02878 = 0.02921 -0.00391 0.00975 0.00031 H19 2 0.479332 0.918800 0.562911 11.00000 0.03625 C20 1 0.338691 0.984718 0.517468 11.00000 0.03785 0.02865 = 0.03363 -0.00724 0.01335 0.00434 H20 2 0.350803 1.062159 0.550985 11.00000 0.05277 C21 1 0.242672 0.959095 0.461241 11.00000 0.03223 0.03133 = 0.02862 0.00177 0.01547 0.01102 C22 1 0.221935 0.851342 0.409966 11.00000 0.02538 0.03407 = 0.02830 -0.00160 0.01137 0.00416 H22 2 0.153336 0.831388 0.370948 11.00000 0.03747 C23 1 0.298294 0.769788 0.415844 11.00000 0.02561 0.02740 = 0.02728 -0.00354 0.01206 0.00138 H23 2 0.282878 0.694584 0.381446 11.00000 0.03145 C24 1 0.073674 1.025275 0.407480 11.00000 0.03569 0.05398 = 0.04551 -0.00260 0.01190 0.02124 H24A 2 0.050180 0.946028 0.424687 11.00000 0.05353 H24B 2 0.064955 1.025094 0.341101 11.00000 0.05289 H24C 2 0.038999 1.092881 0.420328 11.00000 0.04790 O5 5 0.719143 0.950763 0.099408 10.25000 0.02680 0.04220 = 0.03858 0.00586 0.00357 -0.00685 AFIX 3 H5A 2 0.766259 0.901704 0.130626 10.25000 -1.50000 H5B 2 0.667996 0.902764 0.079072 10.25000 -1.50000 AFIX 0 HKLF 4 REM SKM263_0m_a.res in P2(1)/c REM R1 = 0.0349 for 4142 Fo > 4sig(Fo) and 0.0391 for all 4576 data REM 409 parameters refined using 0 restraints END WGHT 0.0389 1.1637 REM Highest difference peak 0.341, deepest hole -0.556, 1-sigma level 0.054 Q1 1 0.8755 0.8313 0.2744 11.00000 0.05 0.34 Q2 1 0.4307 0.7540 0.4783 11.00000 0.05 0.28 Q3 1 0.8112 0.3245 0.4344 11.00000 0.05 0.24 Q4 1 0.7580 0.2793 0.3791 11.00000 0.05 0.24 Q5 1 0.7427 0.3743 0.3996 11.00000 0.05 0.23 ; _shelx_res_checksum 45690 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 S S1 0.45709(2) 0.29846(3) 0.22568(2) 0.02637(11) Uani d 1 . . F F1 0.81951(11) 0.85095(10) 0.24433(11) 0.0709(4) Uani d 1 . . O O1 0.93592(8) 0.24379(11) 0.47803(8) 0.0365(3) Uani d 1 . . O O2 0.88439(7) 0.41670(10) 0.52684(7) 0.0294(2) Uani d 1 . . O O3 0.55706(8) 0.71812(10) 0.54550(7) 0.0307(2) Uani d 1 . . O O4 0.17420(9) 1.04606(11) 0.46165(8) 0.0390(3) Uani d 1 . . N N1 0.64445(8) 0.22708(11) 0.27415(8) 0.0220(2) Uani d 1 . . N N2 0.60560(8) 0.39869(10) 0.34918(8) 0.0200(2) Uani d 1 . . N N3 0.54560(8) 0.55654(10) 0.41266(8) 0.0206(2) Uani d 1 . . N N4 0.46512(8) 0.62737(11) 0.41154(8) 0.0209(2) Uani d 1 . . H H4 0.4182(14) 0.6419(17) 0.3587(13) 0.032(5) Uiso d 1 . . C C1 0.70873(9) 0.43284(13) 0.40035(10) 0.0213(3) Uani d 1 . . H H1 0.7122(12) 0.4512(15) 0.4634(11) 0.022(4) Uiso d 1 . . C C2 0.77324(10) 0.32264(13) 0.39918(10) 0.0224(3) Uani d 1 . . C C3 0.74171(10) 0.23233(13) 0.33574(10) 0.0224(3) Uani d 1 . . C C4 0.58287(10) 0.30597(12) 0.28731(9) 0.0207(3) Uani d 1 . . C C5 0.73684(9) 0.54708(13) 0.35807(10) 0.0233(3) Uani d 1 . . C C6 0.76870(10) 0.65331(14) 0.40974(11) 0.0291(3) Uani d 1 . . H H6 0.7696(14) 0.6545(17) 0.4744(13) 0.035(5) Uiso d 1 . . C C7 0.79756(12) 0.75620(15) 0.37183(14) 0.0365(4) Uani d 1 . . H H7 0.8223(15) 0.829(2) 0.4092(14) 0.048(6) Uiso d 1 . . C C8 0.79149(13) 0.75033(15) 0.28209(14) 0.0410(4) Uani d 1 . . C C9 0.75793(15) 0.64862(16) 0.22793(14) 0.0420(4) Uani d 1 . . H H9 0.7526(16) 0.651(2) 0.1629(15) 0.050(6) Uiso d 1 . . C C10 0.73134(12) 0.54590(14) 0.26730(11) 0.0314(3) Uani d 1 . . H H10 0.7067(14) 0.4745(19) 0.2304(13) 0.038(5) Uiso d 1 . . C C11 0.87186(10) 0.32007(13) 0.46924(10) 0.0253(3) Uani d 1 . . C C12 0.97996(11) 0.42561(17) 0.59855(11) 0.0331(3) Uani d 1 . . H H12A 0.9878(15) 0.353(2) 0.6404(14) 0.045(5) Uiso d 1 . . H H12B 1.0316(14) 0.4216(17) 0.5703(12) 0.034(5) Uiso d 1 . . H H12C 0.9642(16) 0.618(2) 0.6014(15) 0.052(6) Uiso d 1 . . C C13 0.98133(13) 0.5454(2) 0.64668(13) 0.0412(4) Uani d 1 . . H H13A 1.0491(17) 0.557(2) 0.6929(15) 0.055(6) Uiso d 1 . . H H13B 0.9329(18) 0.545(2) 0.6776(16) 0.060(7) Uiso d 1 . . C C14 0.80354(11) 0.12659(15) 0.32406(12) 0.0287(3) Uani d 1 . . H H14A 0.8649(17) 0.155(2) 0.3186(15) 0.052(6) Uiso d 1 . . H H14B 0.8240(16) 0.074(2) 0.3764(16) 0.054(6) Uiso d 1 . . H H14C 0.7663(16) 0.079(2) 0.2696(15) 0.046(5) Uiso d 1 . . C C15 0.52713(9) 0.47098(12) 0.35314(9) 0.0202(3) Uani d 1 . . C C16 0.43099(10) 0.43208(14) 0.28344(10) 0.0260(3) Uani d 1 . . H H16A 0.4032(14) 0.4974(19) 0.2389(13) 0.040(5) Uiso d 1 . . H H16B 0.3839(15) 0.4099(18) 0.3141(14) 0.043(5) Uiso d 1 . . C C17 0.48023(10) 0.71162(13) 0.48039(9) 0.0223(3) Uani d 1 . . C C18 0.39469(10) 0.79431(13) 0.47152(9) 0.0230(3) Uani d 1 . . C C19 0.41359(12) 0.90278(14) 0.52329(10) 0.0289(3) Uani d 1 . . H H19 0.4793(15) 0.9188(17) 0.5629(13) 0.036(5) Uiso d 1 . . C C20 0.33869(12) 0.98472(15) 0.51747(11) 0.0331(3) Uani d 1 . . H H20 0.3508(16) 1.062(2) 0.5510(15) 0.053(6) Uiso d 1 . . C C21 0.24267(11) 0.95909(15) 0.46124(10) 0.0294(3) Uani d 1 . . C C22 0.22193(11) 0.85134(15) 0.40997(10) 0.0287(3) Uani d 1 . . H H22 0.1533(15) 0.8314(18) 0.3709(13) 0.037(5) Uiso d 1 . . C C23 0.29829(11) 0.76979(14) 0.41584(10) 0.0260(3) Uani d 1 . . H H23 0.2829(13) 0.6946(17) 0.3814(12) 0.031(5) Uiso d 1 . . C C24 0.07367(14) 1.0253(2) 0.40748(14) 0.0456(5) Uani d 1 . . H H24A 0.0502(16) 0.946(2) 0.4247(15) 0.054(6) Uiso d 1 . . H H24B 0.0650(16) 1.025(2) 0.3411(16) 0.053(6) Uiso d 1 . . H H24C 0.0390(16) 1.093(2) 0.4203(14) 0.048(6) Uiso d 1 . . O O5 0.7191(3) 0.9508(5) 0.0994(3) 0.0378(10) Uani d 0.25 . . H H5A 0.766259 0.901704 0.130626 0.057 Uiso d 0.25 . . H H5B 0.667996 0.902764 0.079072 0.057 Uiso d 0.25 . . 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 0.01757(17) 0.0260(2) 0.0312(2) 0.00125(12) 0.00266(13) -0.00720(13) F1 0.1061(11) 0.0263(6) 0.1191(11) -0.0171(6) 0.0888(10) -0.0055(6) O1 0.0214(5) 0.0345(6) 0.0476(7) 0.0093(4) 0.0038(5) -0.0055(5) O2 0.0177(5) 0.0313(6) 0.0326(6) 0.0026(4) 0.0002(4) -0.0057(4) O3 0.0271(5) 0.0336(6) 0.0274(5) 0.0038(4) 0.0040(4) -0.0039(4) O4 0.0370(6) 0.0405(7) 0.0400(6) 0.0175(5) 0.0137(5) -0.0051(5) N1 0.0198(5) 0.0194(6) 0.0257(6) 0.0010(4) 0.0064(5) -0.0013(4) N2 0.0151(5) 0.0186(6) 0.0246(6) 0.0011(4) 0.0046(4) -0.0013(4) N3 0.0174(5) 0.0202(6) 0.0246(6) 0.0028(4) 0.0078(4) 0.0011(4) N4 0.0179(5) 0.0216(6) 0.0231(6) 0.0044(4) 0.0069(5) 0.0005(4) C1 0.0151(6) 0.0211(7) 0.0256(7) 0.0001(5) 0.0042(5) -0.0028(5) C2 0.0169(6) 0.0208(7) 0.0284(7) 0.0019(5) 0.0062(5) 0.0005(5) C3 0.0190(6) 0.0205(7) 0.0276(7) 0.0016(5) 0.0079(5) 0.0023(5) C4 0.0206(6) 0.0181(7) 0.0230(7) -0.0001(5) 0.0067(5) 0.0005(5) C5 0.0146(6) 0.0199(7) 0.0348(8) 0.0012(5) 0.0077(5) -0.0021(5) C6 0.0207(7) 0.0237(8) 0.0399(9) 0.0007(5) 0.0066(6) -0.0057(6) C7 0.0270(8) 0.0204(8) 0.0640(11) -0.0040(6) 0.0179(8) -0.0093(7) C8 0.0439(9) 0.0204(8) 0.0744(13) -0.0032(7) 0.0406(9) 0.0001(8) C9 0.0582(11) 0.0270(9) 0.0568(11) -0.0018(7) 0.0402(10) -0.0014(7) C10 0.0373(8) 0.0227(8) 0.0403(9) -0.0035(6) 0.0212(7) -0.0051(6) C11 0.0191(6) 0.0238(7) 0.0312(7) 0.0015(5) 0.0064(6) -0.0005(6) C12 0.0177(7) 0.0431(10) 0.0315(8) 0.0004(6) -0.0005(6) -0.0031(7) C13 0.0284(8) 0.0560(12) 0.0348(9) -0.0025(8) 0.0053(7) -0.0140(8) C14 0.0239(7) 0.0252(8) 0.0356(8) 0.0050(6) 0.0083(6) -0.0037(6) C15 0.0171(6) 0.0186(7) 0.0246(7) 0.0011(5) 0.0068(5) 0.0028(5) C16 0.0187(6) 0.0254(8) 0.0303(8) 0.0020(5) 0.0038(6) -0.0048(6) C17 0.0226(7) 0.0217(7) 0.0234(7) 0.0007(5) 0.0090(5) 0.0015(5) C18 0.0246(7) 0.0235(7) 0.0234(7) 0.0023(5) 0.0113(6) 0.0002(5) C19 0.0287(8) 0.0288(8) 0.0292(8) 0.0003(6) 0.0098(6) -0.0039(6) C20 0.0378(9) 0.0286(8) 0.0336(8) 0.0043(6) 0.0134(7) -0.0072(6) C21 0.0322(8) 0.0313(8) 0.0286(8) 0.0110(6) 0.0155(6) 0.0018(6) C22 0.0254(7) 0.0341(8) 0.0283(7) 0.0042(6) 0.0114(6) -0.0016(6) C23 0.0256(7) 0.0274(8) 0.0273(7) 0.0014(6) 0.0121(6) -0.0035(6) C24 0.0357(9) 0.0540(12) 0.0455(11) 0.0212(9) 0.0119(8) -0.0026(9) O5 0.027(2) 0.042(3) 0.039(3) -0.0069(19) 0.0036(19) 0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 C4 S1 C16 . . 92.44(6) ? C11 O2 C12 . . 116.09(11) ? C21 O4 C24 . . 118.60(14) ? C4 N1 C3 . . 116.27(12) ? C4 N2 C15 . . 116.48(11) ? C4 N2 C1 . . 121.74(11) ? C15 N2 C1 . . 121.23(11) ? C15 N3 N4 . . 115.33(11) ? C17 N4 N3 . . 116.80(11) ? C17 N4 H4 . . 118.6(12) ? N3 N4 H4 . . 118.8(12) ? N2 C1 C2 . . 107.75(11) ? N2 C1 C5 . . 109.80(11) ? C2 C1 C5 . . 112.38(11) ? N2 C1 H1 . . 106.8(9) ? C2 C1 H1 . . 110.3(9) ? C5 C1 H1 . . 109.6(10) ? C3 C2 C11 . . 121.84(12) ? C3 C2 C1 . . 121.53(12) ? C11 C2 C1 . . 116.62(12) ? C2 C3 N1 . . 122.42(12) ? C2 C3 C14 . . 125.10(13) ? N1 C3 C14 . . 112.47(12) ? N1 C4 N2 . . 126.10(12) ? N1 C4 S1 . . 121.47(10) ? N2 C4 S1 . . 112.41(10) ? C10 C5 C6 . . 119.33(14) ? C10 C5 C1 . . 120.14(13) ? C6 C5 C1 . . 120.53(13) ? C5 C6 C7 . . 120.41(16) ? C5 C6 H6 . . 118.7(11) ? C7 C6 H6 . . 120.9(11) ? C8 C7 C6 . . 118.11(15) ? C8 C7 H7 . . 122.1(12) ? C6 C7 H7 . . 119.8(12) ? F1 C8 C7 . . 118.48(16) ? F1 C8 C9 . . 118.13(17) ? C7 C8 C9 . . 123.39(16) ? C8 C9 C10 . . 117.76(17) ? C8 C9 H9 . . 119.7(13) ? C10 C9 H9 . . 122.5(13) ? C9 C10 C5 . . 120.96(15) ? C9 C10 H10 . . 119.1(12) ? C5 C10 H10 . . 119.9(12) ? O1 C11 O2 . . 122.00(13) ? O1 C11 C2 . . 127.18(14) ? O2 C11 C2 . . 110.81(11) ? O2 C12 C13 . . 106.88(13) ? O2 C12 H12A . . 108.3(12) ? C13 C12 H12A . . 112.1(12) ? O2 C12 H12B . . 108.5(11) ? C13 C12 H12B . . 112.3(11) ? H12A C12 H12B . . 108.7(16) ? C12 C13 H12C . . 111.3(12) ? C12 C13 H13A . . 107.9(13) ? H12C C13 H13A . . 110.2(18) ? C12 C13 H13B . . 110.9(14) ? H12C C13 H13B . . 107.1(18) ? H13A C13 H13B . . 109.4(19) ? C3 C14 H14A . . 111.4(13) ? C3 C14 H14B . . 112.1(14) ? H14A C14 H14B . . 103.9(18) ? C3 C14 H14C . . 109.4(12) ? H14A C14 H14C . . 109.8(18) ? H14B C14 H14C . . 110.1(18) ? N3 C15 N2 . . 118.03(12) ? N3 C15 C16 . . 130.06(12) ? N2 C15 C16 . . 111.90(11) ? C15 C16 S1 . . 106.69(9) ? C15 C16 H16A . . 111.4(12) ? S1 C16 H16A . . 109.4(11) ? C15 C16 H16B . . 109.7(12) ? S1 C16 H16B . . 109.9(12) ? H16A C16 H16B . . 109.8(16) ? O3 C17 N4 . . 123.09(13) ? O3 C17 C18 . . 121.90(13) ? N4 C17 C18 . . 115.00(12) ? C23 C18 C19 . . 118.49(13) ? C23 C18 C17 . . 124.17(13) ? C19 C18 C17 . . 117.34(13) ? C20 C19 C18 . . 120.67(15) ? C20 C19 H19 . . 120.6(11) ? C18 C19 H19 . . 118.8(11) ? C19 C20 C21 . . 120.16(15) ? C19 C20 H20 . . 121.9(13) ? C21 C20 H20 . . 117.9(13) ? O4 C21 C22 . . 124.66(14) ? O4 C21 C20 . . 115.13(14) ? C22 C21 C20 . . 120.20(14) ? C21 C22 C23 . . 119.12(14) ? C21 C22 H22 . . 120.7(11) ? C23 C22 H22 . . 120.2(11) ? C18 C23 C22 . . 121.34(14) ? C18 C23 H23 . . 120.2(11) ? C22 C23 H23 . . 118.4(11) ? O4 C24 H24A . . 110.4(13) ? O4 C24 H24B . . 110.9(13) ? H24A C24 H24B . . 110.1(18) ? O4 C24 H24C . . 104.9(13) ? H24A C24 H24C . . 111.1(18) ? H24B C24 H24C . . 109.4(18) ? H5A O5 H5B . . 104.0 ? 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 C4 . 1.7422(14) ? S1 C16 . 1.8130(15) ? F1 C8 . 1.3657(19) ? O1 C11 . 1.2133(18) ? O2 C11 . 1.3522(18) ? O2 C12 . 1.4526(17) ? O3 C17 . 1.2236(17) ? O4 C21 . 1.3680(18) ? O4 C24 . 1.426(2) ? N1 C4 . 1.2996(18) ? N1 C3 . 1.4058(17) ? N2 C4 . 1.3546(17) ? N2 C15 . 1.3963(17) ? N2 C1 . 1.4762(16) ? N3 C15 . 1.2750(18) ? N3 N4 . 1.3880(15) ? N4 C17 . 1.3698(18) ? N4 H4 . 0.885(19) ? C1 C2 . 1.5194(18) ? C1 C5 . 1.5226(19) ? C1 H1 . 0.987(17) ? C2 C3 . 1.356(2) ? C2 C11 . 1.4694(19) ? C3 C14 . 1.5024(19) ? C5 C10 . 1.391(2) ? C5 C6 . 1.392(2) ? C6 C7 . 1.392(2) ? C6 H6 . 1.004(19) ? C7 C8 . 1.373(3) ? C7 H7 . 0.97(2) ? C8 C9 . 1.374(3) ? C9 C10 . 1.388(2) ? C9 H9 . 0.99(2) ? C10 H10 . 0.96(2) ? C12 C13 . 1.498(2) ? C12 H12A . 1.00(2) ? C12 H12B . 0.988(19) ? C13 H12C . 1.03(2) ? C13 H13A . 1.00(2) ? C13 H13B . 0.98(3) ? C14 H14A . 0.97(2) ? C14 H14B . 0.96(2) ? C14 H14C . 0.98(2) ? C15 C16 . 1.5020(19) ? C16 H16A . 0.98(2) ? C16 H16B . 0.98(2) ? C17 C18 . 1.4939(19) ? C18 C23 . 1.391(2) ? C18 C19 . 1.401(2) ? C19 C20 . 1.379(2) ? C19 H19 . 0.96(2) ? C20 C21 . 1.392(2) ? C20 H20 . 0.97(2) ? C21 C22 . 1.390(2) ? C22 C23 . 1.392(2) ? C22 H22 . 0.99(2) ? C23 H23 . 0.960(19) ? C24 H24A . 0.99(2) ? C24 H24B . 1.00(2) ? C24 H24C . 0.95(2) ? O5 H5A . 0.8700 ? O5 H5B . 0.8701 ? 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 N4 H4 N1 2_655 0.885(19) 2.164(19) 2.9888(17) 154.8(16) yes C1 H1 O5 4_576 0.987(17) 2.345(18) 3.307(5) 164.7(13) yes C7 H7 O4 3_676 0.97(2) 2.41(2) 3.285(2) 148.7(17) yes C13 H13B F1 4_576 0.98(3) 2.49(3) 3.386(2) 153.0(19) yes C16 H16A N1 2_655 0.98(2) 2.58(2) 3.4019(19) 142.4(15) yes C16 H16B O5 2_645 0.98(2) 2.37(2) 3.282(5) 154.6(16) yes C24 H24A O1 3_666 0.99(2) 2.53(2) 3.450(3) 154.6(18) yes C24 H24C O1 1_465 0.95(2) 2.57(2) 3.504(2) 167.8(17) yes O5 H5A F1 . 0.87 1.76 2.479(5) 138 yes O5 H5B O3 4_575 0.87 2.00 2.863(5) 174 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 C15 N3 N4 C17 . . . . 173.45(12) ? C4 N2 C1 C2 . . . . -21.62(17) ? C15 N2 C1 C2 . . . . 167.22(11) ? C4 N2 C1 C5 . . . . 101.08(14) ? C15 N2 C1 C5 . . . . -70.08(15) ? N2 C1 C2 C3 . . . . 20.41(18) ? C5 C1 C2 C3 . . . . -100.69(15) ? N2 C1 C2 C11 . . . . -160.54(12) ? C5 C1 C2 C11 . . . . 78.36(15) ? C11 C2 C3 N1 . . . . 173.50(13) ? C1 C2 C3 N1 . . . . -7.5(2) ? C11 C2 C3 C14 . . . . -5.0(2) ? C1 C2 C3 C14 . . . . 174.03(14) ? C4 N1 C3 C2 . . . . -7.2(2) ? C4 N1 C3 C14 . . . . 171.48(13) ? C3 N1 C4 N2 . . . . 6.2(2) ? C3 N1 C4 S1 . . . . -171.99(10) ? C15 N2 C4 N1 . . . . -178.53(13) ? C1 N2 C4 N1 . . . . 9.9(2) ? C15 N2 C4 S1 . . . . -0.18(15) ? C1 N2 C4 S1 . . . . -171.74(10) ? C16 S1 C4 N1 . . . . -179.84(12) ? C16 S1 C4 N2 . . . . 1.73(11) ? N2 C1 C5 C10 . . . . -58.95(16) ? C2 C1 C5 C10 . . . . 60.97(17) ? N2 C1 C5 C6 . . . . 121.37(13) ? C2 C1 C5 C6 . . . . -118.72(14) ? C10 C5 C6 C7 . . . . -1.9(2) ? C1 C5 C6 C7 . . . . 177.79(13) ? C5 C6 C7 C8 . . . . 1.4(2) ? C6 C7 C8 F1 . . . . 179.90(15) ? C6 C7 C8 C9 . . . . 0.4(3) ? F1 C8 C9 C10 . . . . 178.81(16) ? C7 C8 C9 C10 . . . . -1.7(3) ? C8 C9 C10 C5 . . . . 1.2(3) ? C6 C5 C10 C9 . . . . 0.6(2) ? C1 C5 C10 C9 . . . . -179.13(15) ? C12 O2 C11 O1 . . . . 1.5(2) ? C12 O2 C11 C2 . . . . -179.00(12) ? C3 C2 C11 O1 . . . . 2.3(2) ? C1 C2 C11 O1 . . . . -176.78(15) ? C3 C2 C11 O2 . . . . -177.21(13) ? C1 C2 C11 O2 . . . . 3.75(18) ? C11 O2 C12 C13 . . . . 173.66(14) ? N4 N3 C15 N2 . . . . 178.26(11) ? N4 N3 C15 C16 . . . . -2.1(2) ? C4 N2 C15 N3 . . . . 177.79(12) ? C1 N2 C15 N3 . . . . -10.60(19) ? C4 N2 C15 C16 . . . . -1.93(17) ? C1 N2 C15 C16 . . . . 169.67(12) ? N3 C15 C16 S1 . . . . -176.70(12) ? N2 C15 C16 S1 . . . . 2.98(14) ? C4 S1 C16 C15 . . . . -2.61(11) ? N3 N4 C17 O3 . . . . -7.08(19) ? N3 N4 C17 C18 . . . . 174.20(11) ? O3 C17 C18 C23 . . . . -160.50(14) ? N4 C17 C18 C23 . . . . 18.2(2) ? O3 C17 C18 C19 . . . . 19.1(2) ? N4 C17 C18 C19 . . . . -162.14(13) ? C23 C18 C19 C20 . . . . -1.5(2) ? C17 C18 C19 C20 . . . . 178.83(14) ? C18 C19 C20 C21 . . . . 1.3(2) ? C24 O4 C21 C22 . . . . 1.3(2) ? C24 O4 C21 C20 . . . . -178.54(16) ? C19 C20 C21 O4 . . . . 179.23(14) ? C19 C20 C21 C22 . . . . -0.6(2) ? O4 C21 C22 C23 . . . . -179.73(14) ? C20 C21 C22 C23 . . . . 0.1(2) ? C19 C18 C23 C22 . . . . 1.0(2) ? C17 C18 C23 C22 . . . . -179.37(13) ? C21 C22 C23 C18 . . . . -0.3(2) ? _cod_database_fobs_code 2244141