#------------------------------------------------------------------------------ #$Date: 2024-08-07 01:05:40 +0300 (Wed, 07 Aug 2024) $ #$Revision: 293996 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/31/2023178.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_2023178 loop_ _publ_author_name 'Mustaphi, Nour El Hoda' 'Chlouchi, Amina' 'El Hafi, Mohamed' 'Mague, Joel T.' 'Hökelek, Tuncer' 'El Monfalouti, Hanae' 'Haoudi, Amal' 'Mazzah, Ahmed' _publ_section_title ; Crystal structure determination and analyses of Hirshfeld surface, crystal voids, inter-molecular inter-action energies and energy frameworks of 1-benzyl-4-(methyl-sulfan-yl)-3a,7a-di-hydro-1H-pyrazolo-[3,4-d]pyrimidine. ; _journal_coeditor_code WM5721 _journal_issue 'Pt 7' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 783 _journal_page_last 788 _journal_paper_doi 10.1107/S2056989024005954 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C13 H12 N4 S' _chemical_formula_moiety 'C13 H12 N4 S' _chemical_formula_sum 'C13 H12 N4 S' _chemical_formula_weight 256.33 _chemical_name_systematic 1-Benzyl-4-(methylsulfanyl)-3a,7a-dihydro-1H-pyrazolo[3,4-d]pyrimidine _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 dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 96.0850(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.4617(5) _cell_length_b 7.0766(3) _cell_length_c 13.6500(5) _cell_measurement_reflns_used 7875 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 74.7271 _cell_measurement_theta_min 6.2542 _cell_volume 1196.96(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 ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4167 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.976 _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 0.0261 _diffrn_reflns_av_unetI/netI 0.0248 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 8877 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 74.719 _diffrn_reflns_theta_min 6.522 _diffrn_source 'INCOATEC I\mS micro--focus source' _exptl_absorpt_coefficient_mu 2.285 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.257 _exptl_crystal_size_mid 0.218 _exptl_crystal_size_min 0.156 _refine_diff_density_max 0.684 _refine_diff_density_min -0.419 _refine_ls_extinction_coef 0.0175(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2018/3 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 2388 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0487 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0792P)^2^+0.9126P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1338 _refine_ls_wR_factor_ref 0.1349 _reflns_number_gt 2292 _reflns_number_total 2388 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm5721.cif _cod_data_source_block I _cod_depositor_comments 'Adding full bibliography for 2023178.cif.' _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2023178 _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 0.591 _shelx_estimated_absorpt_t_max 0.717 _shelx_hkl_file ; 2 0 0 208.08 7.50 -2 0 0 225.98 7.50 -3 0 0 1010.60 33.20 3 0 0 981.00 33.20 4 0 0 526.85 18.10 5 0 0 3305.77 110.09 -5 0 0 3419.86 110.19 5 0 0 3258.07 109.39 6 0 0 242.68 8.70 6 0 0 243.68 9.50 -6 0 0 241.08 9.60 7 0 0 614.24 20.70 7 0 0 596.54 21.90 8 0 0 141.79 5.60 8 0 0 130.19 5.40 9 0 0 57.79 3.10 9 0 0 61.89 2.90 10 0 0 150.58 6.00 10 0 0 152.58 6.40 11 0 0 231.48 9.80 11 0 0 246.88 8.90 12 0 0 252.67 10.20 12 0 0 269.77 9.60 13 0 0 440.16 15.80 14 0 0 15.50 1.70 0 -1 0 0.90 0.30 0 1 0 0.70 0.30 1 -1 0 2428.66 76.39 -1 -1 0 2217.28 76.39 -2 -1 0 507.15 17.60 2 -1 0 514.65 17.70 -2 1 0 547.45 17.70 -3 -1 0 1.60 0.50 3 -1 0 1.70 0.60 -3 1 0 1.60 0.70 -4 -1 0 265.27 9.60 4 -1 0 274.67 9.70 -4 1 0 269.27 9.80 4 1 0 251.47 9.60 -5 -1 0 343.17 12.00 5 -1 0 323.67 11.60 5 1 0 315.57 11.30 -5 1 0 325.27 12.10 5 1 0 316.17 11.90 6 -1 0 128.09 5.00 6 -1 0 137.39 5.90 -6 -1 0 120.69 5.80 -6 1 0 122.89 6.00 6 1 0 125.89 5.00 6 1 0 125.79 5.70 7 -1 0 346.27 11.90 7 -1 0 332.97 13.20 7 1 0 326.27 13.20 7 1 0 338.07 12.00 8 -1 0 126.69 4.90 8 -1 0 114.09 4.70 8 1 0 107.09 4.70 8 1 0 115.89 4.90 9 -1 0 101.79 4.60 9 -1 0 101.19 4.40 9 1 0 112.39 4.80 9 1 0 105.59 4.40 10 -1 0 10.70 1.50 10 -1 0 8.90 1.50 10 1 0 10.30 1.70 10 1 0 11.80 1.40 11 -1 0 5.80 1.40 11 -1 0 6.20 1.50 11 1 0 7.40 1.40 11 1 0 5.70 1.50 -11 1 0 4.10 1.20 12 -1 0 212.88 8.50 -12 1 0 219.88 8.00 12 1 0 217.18 8.70 12 1 0 222.08 8.10 13 -1 0 40.90 2.60 13 1 0 40.70 3.10 14 -1 0 73.19 3.50 14 1 0 69.89 3.40 -15 1 0 0.10 0.50 0 -2 0 984.90 33.30 0 2 0 1001.40 33.30 1 -2 0 2651.23 91.29 -1 -2 0 2882.81 91.39 2 -2 0 1657.23 57.19 -2 -2 0 1761.12 57.19 -2 2 0 1742.53 57.39 3 -2 0 944.71 32.00 -3 -2 0 911.71 31.90 -3 -2 0 972.60 31.90 -3 2 0 937.61 32.10 4 -2 0 288.57 10.70 -4 -2 0 285.27 10.60 -4 2 0 280.37 10.90 5 -2 0 463.65 16.50 -5 -2 0 450.35 16.40 5 -2 0 435.36 15.40 -5 2 0 425.86 16.60 5 2 0 479.65 15.60 6 -2 0 36.30 2.20 6 -2 0 42.40 3.20 6 2 0 32.30 2.10 7 -2 0 548.15 18.70 7 -2 0 533.35 18.60 7 2 0 546.95 18.90 8 -2 0 18.20 1.90 8 -2 0 19.30 1.80 8 2 0 16.80 2.00 8 2 0 23.00 1.90 9 -2 0 426.96 14.50 9 -2 0 385.96 15.10 9 2 0 391.16 14.10 9 2 0 414.76 14.70 -9 2 0 399.76 14.10 10 -2 0 700.03 24.20 10 -2 0 707.73 24.00 10 2 0 688.93 23.80 10 2 0 715.13 24.40 -10 2 0 680.83 23.70 11 -2 0 193.88 7.50 11 2 0 183.38 7.00 11 2 0 173.68 7.50 -11 2 0 190.48 7.00 12 -2 0 50.79 3.00 12 2 0 51.19 3.60 12 2 0 46.90 2.90 13 -2 0 72.39 3.80 -13 2 0 82.29 3.90 13 2 0 77.89 3.90 14 2 0 193.98 7.50 -14 2 0 199.78 7.10 -15 2 0 2.50 0.80 0 -3 0 1.50 0.80 0 3 0 2.50 0.90 1 -3 0 523.75 18.00 -1 -3 0 500.25 18.30 -1 3 0 497.85 18.20 2 -3 0 58.59 3.30 -2 -3 0 61.09 3.30 -2 3 0 59.09 3.60 -3 -3 0 664.33 23.00 3 -3 0 638.24 22.80 -3 -3 0 683.33 22.90 -3 3 0 597.44 23.10 -4 -3 0 10.60 2.60 4 -3 0 8.20 1.80 -4 -3 0 5.00 2.20 4 3 0 7.50 1.40 5 -3 0 721.43 26.30 -5 -3 0 736.03 26.30 5 3 0 739.33 24.90 -6 -3 0 8.10 3.90 6 -3 0 7.50 2.00 6 3 0 5.60 1.30 -6 3 0 5.90 1.10 7 -3 0 192.08 7.60 -7 3 0 201.38 7.40 7 3 0 208.18 7.80 8 -3 0 79.89 4.00 -8 3 0 82.69 3.70 8 3 0 87.69 4.10 9 -3 0 51.79 3.20 9 3 0 54.79 3.10 -9 3 0 49.70 2.70 9 3 0 53.29 3.10 10 -3 0 136.99 5.90 10 3 0 131.79 5.40 10 3 0 129.79 5.80 -10 3 0 136.79 5.30 11 3 0 528.25 18.10 11 3 0 499.15 18.70 -11 3 0 552.84 18.20 12 3 0 489.65 17.80 -12 3 0 513.45 17.20 13 3 0 24.40 2.00 -13 3 0 26.60 1.60 -13 3 0 25.10 1.80 -14 3 0 139.29 5.10 0 -4 0 443.56 16.70 1 -4 0 13.60 3.00 -1 -4 0 19.00 2.70 -2 -4 0 140.89 6.70 2 -4 0 124.49 6.60 -3 -4 0 873.71 30.80 3 4 0 853.61 29.10 3 4 0 878.71 29.00 -3 4 0 835.02 28.90 4 4 0 36.50 2.30 -4 4 0 33.30 2.10 -4 4 0 29.40 2.70 4 4 0 33.60 2.80 -5 4 0 1.70 0.80 5 4 0 -0.10 1.40 -5 4 0 3.10 1.50 5 4 0 1.40 1.10 5 4 0 0.90 1.10 -5 4 0 1.70 1.50 -6 4 0 4.20 1.40 -6 4 0 6.30 2.80 6 4 0 4.80 1.30 -6 4 0 6.60 1.30 6 4 0 4.10 1.20 6 4 0 2.40 1.60 7 4 0 8.20 2.10 7 4 0 3.40 1.30 -7 4 0 1.30 0.80 8 4 0 224.48 8.80 -8 4 0 220.18 8.30 -9 4 0 342.77 12.50 9 4 0 348.87 13.00 -9 4 0 365.96 12.70 -10 4 0 75.59 3.50 10 4 0 69.89 3.80 -10 4 0 75.79 3.40 -11 4 0 0.80 0.70 -11 4 0 0.70 0.80 11 4 0 0.20 1.30 -12 4 0 12.50 1.30 12 4 0 7.90 2.10 -12 4 0 11.50 1.20 -13 4 0 -0.80 0.70 -13 4 0 -0.10 0.80 0 5 0 1.20 1.10 0 5 0 3.40 1.20 0 5 0 1.20 1.00 1 5 0 597.84 20.50 -1 5 0 599.04 20.50 -1 5 0 594.94 20.50 1 5 0 613.04 20.60 -1 5 0 564.14 20.60 1 5 0 628.24 20.60 2 5 0 904.21 30.40 -2 5 0 884.11 30.40 2 5 0 921.91 30.60 -2 5 0 920.61 30.50 -2 5 0 840.52 30.40 2 5 0 951.30 30.60 -3 5 0 228.48 8.80 3 5 0 245.18 8.80 -3 5 0 227.88 8.60 3 5 0 244.98 8.70 3 5 0 222.38 8.70 -3 5 0 237.68 8.70 -4 5 0 38.90 3.50 4 5 0 48.10 3.00 -4 5 0 48.30 2.70 -4 5 0 49.70 2.80 4 5 0 49.10 2.70 5 5 0 254.37 9.30 5 5 0 253.67 9.20 -5 5 0 242.38 9.60 -5 5 0 245.28 9.20 6 5 0 2.00 1.20 -6 5 0 0.80 0.80 -6 5 0 2.80 1.40 -6 5 0 2.60 1.60 7 5 0 3.60 1.20 -7 5 0 3.30 1.50 -7 5 0 1.20 0.80 7 5 0 1.00 1.30 -8 5 0 8.80 1.40 -8 5 0 11.00 2.20 8 5 0 7.10 2.00 -9 5 0 8.40 1.30 -9 5 0 6.70 1.30 -10 5 0 6.80 1.10 -10 5 0 7.80 1.60 -11 5 0 501.45 17.10 -11 5 0 501.85 17.10 -12 5 0 231.08 7.90 -12 5 0 225.38 8.00 0 6 0 602.24 21.00 0 6 0 610.14 21.00 0 6 0 615.14 20.90 1 6 0 165.68 6.40 -1 6 0 158.08 6.50 -1 6 0 163.78 6.40 1 6 0 162.58 6.60 1 6 0 167.68 6.40 -1 6 0 159.48 6.40 2 6 0 154.58 6.20 2 6 0 156.48 6.00 -2 6 0 143.69 6.10 -2 6 0 150.38 6.00 -2 6 0 148.49 6.00 2 6 0 155.68 6.20 -3 6 0 151.78 6.10 -3 6 0 153.28 6.30 -3 6 0 149.49 6.10 3 6 0 159.58 6.30 3 6 0 155.18 6.10 4 6 0 54.19 3.10 -4 6 0 51.89 2.80 4 6 0 55.49 2.90 -4 6 0 57.49 2.90 -4 6 0 50.29 3.40 -5 6 0 87.89 4.00 -5 6 0 87.19 4.00 5 6 0 90.59 4.00 5 6 0 90.19 4.20 6 6 0 96.89 4.30 -6 6 0 92.19 4.20 6 6 0 99.19 4.20 -7 6 0 198.88 7.70 7 6 0 179.58 7.00 7 6 0 183.98 7.10 -8 6 0 0.50 0.60 8 6 0 -0.10 1.10 -9 6 0 86.09 3.60 -10 6 0 136.59 5.10 -11 6 0 14.70 1.10 0 7 0 2.10 1.00 0 7 0 0.00 0.90 0 7 0 -0.70 0.70 -1 7 0 70.89 3.40 -1 7 0 73.49 3.60 1 7 0 74.89 3.40 -1 7 0 69.99 3.40 1 7 0 71.89 3.50 1 7 0 66.59 4.10 -2 7 0 54.69 2.90 -2 7 0 59.59 3.10 -2 7 0 54.69 2.90 2 7 0 60.49 3.00 2 7 0 61.89 3.10 -3 7 0 29.10 2.60 -3 7 0 33.50 2.20 -3 7 0 33.80 2.50 3 7 0 39.00 2.40 3 7 0 39.00 2.20 4 7 0 28.80 1.80 -4 7 0 21.80 1.70 4 7 0 25.00 2.00 -4 7 0 20.70 2.60 -4 7 0 22.40 1.70 5 7 0 91.79 3.90 5 7 0 96.29 4.10 -5 7 0 94.49 4.00 -6 7 0 56.79 2.70 6 7 0 59.29 2.70 6 7 0 63.69 2.90 7 7 0 15.50 1.30 -7 7 0 14.90 1.20 7 7 0 16.50 1.70 -8 7 0 1.30 0.60 -9 7 0 3.70 0.70 0 8 0 500.25 16.90 0 8 0 472.35 16.60 -1 8 0 174.18 6.50 -1 8 0 183.98 6.60 -1 8 0 180.78 6.60 1 8 0 181.18 6.70 1 8 0 184.98 6.80 -2 8 0 135.69 5.20 -2 8 0 134.39 5.20 2 8 0 144.99 5.30 2 8 0 138.19 5.40 -2 8 0 137.29 5.10 3 8 0 1.50 0.70 3 8 0 4.60 0.90 -3 8 0 2.90 0.70 -3 8 0 3.10 1.10 4 8 0 387.56 13.20 -4 8 0 372.66 13.20 4 8 0 395.26 13.20 -5 8 0 1.30 0.60 5 8 0 0.80 0.60 5 8 0 1.90 0.70 6 8 0 85.19 3.50 -6 8 0 74.59 3.00 14 0 -1 -1.20 0.90 13 0 -1 0.00 0.90 13 0 -1 0.50 0.60 12 0 -1 -0.60 0.80 12 0 -1 0.80 0.90 11 0 -1 1.30 0.70 10 0 -1 0.10 0.60 10 0 -1 0.60 0.80 9 0 -1 1.10 0.80 9 0 -1 0.00 0.70 9 0 -1 -0.60 1.00 8 0 -1 0.40 0.70 8 0 -1 0.90 0.90 8 0 -1 0.80 1.90 7 0 -1 0.90 1.10 -7 0 1 0.50 2.30 7 0 -1 1.40 0.70 -6 0 1 1.30 0.90 6 0 -1 2.00 0.70 6 0 -1 1.20 0.80 -5 0 1 0.70 0.50 5 0 -1 0.80 0.60 5 0 -1 1.30 0.80 4 0 -1 0.10 0.30 -4 0 1 0.30 0.40 3 0 -1 0.30 0.20 -3 0 1 0.30 0.30 1 0 -1 0.40 0.10 -1 0 1 0.60 0.10 0 0 -1 0.50 0.10 1 0 1 0.10 0.10 -1 0 -1 0.10 0.10 -2 0 -1 1.00 0.40 3 0 1 0.20 0.20 -3 0 -1 0.40 0.30 4 0 1 -0.10 0.30 -4 0 -1 0.90 0.50 5 0 1 1.90 0.70 5 0 1 2.10 1.00 -5 0 -1 2.90 1.20 6 0 1 1.90 0.70 6 0 1 1.00 0.90 -6 0 -1 1.10 1.20 7 0 1 2.70 0.80 7 0 1 1.00 1.30 8 0 1 0.20 0.60 8 0 1 0.90 0.90 9 0 1 -0.80 0.70 9 0 1 0.90 0.80 10 0 1 -0.10 0.90 10 0 1 -0.30 0.80 11 0 1 0.00 0.80 11 0 1 1.20 0.90 12 0 1 0.30 0.90 13 0 1 0.90 0.90 14 0 1 0.00 1.00 -15 0 -1 0.10 0.60 14 -1 -1 374.76 13.20 14 1 -1 364.46 13.20 13 -1 -1 5.20 1.40 13 1 -1 3.40 1.10 -13 1 1 1.50 1.10 13 1 -1 2.10 0.90 12 -1 -1 111.09 4.50 12 -1 -1 100.19 4.80 12 1 -1 93.19 4.70 -12 1 1 110.69 4.40 12 1 -1 105.29 4.40 11 -1 -1 1197.58 38.90 11 -1 -1 1137.69 39.10 11 1 -1 1117.99 39.20 11 1 -1 1157.68 38.70 10 -1 -1 988.00 33.10 10 -1 -1 960.50 32.70 10 1 -1 985.50 33.50 10 1 -1 943.61 32.70 9 -1 -1 218.68 8.40 9 1 -1 230.18 8.50 9 1 -1 223.18 8.10 9 1 -1 205.18 8.00 8 -1 -1 891.61 32.30 8 -1 -1 1009.30 32.60 8 1 -1 1000.10 32.70 8 1 -1 953.60 32.30 7 -1 -1 790.32 28.20 7 -1 -1 798.42 27.00 7 1 -1 802.42 27.10 7 1 -1 805.32 28.20 6 -1 -1 878.81 29.20 -6 -1 1 815.12 28.90 6 -1 -1 858.81 28.20 6 1 -1 856.81 28.30 -6 1 1 786.52 29.10 6 1 -1 839.62 29.00 5 -1 -1 64.59 2.80 -5 -1 1 63.59 3.10 5 -1 -1 65.29 3.20 5 1 -1 60.09 3.10 5 1 -1 61.19 2.80 -5 1 1 66.79 3.30 -4 -1 1 134.89 5.00 4 -1 -1 129.69 5.10 4 1 -1 124.69 5.00 -4 1 1 122.69 5.10 3 -1 -1 3132.09 103.19 -2 -1 1 32.50 1.40 2 -1 -1 28.60 1.50 -2 1 1 29.80 1.50 1 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5.80 1.50 -7 0 -6 3.10 1.40 7 0 6 5.30 1.60 -8 0 -6 3237.18 109.29 8 0 6 3331.57 109.29 8 0 6 3369.06 109.79 9 0 6 6.20 1.70 -9 0 -6 10.70 1.90 10 0 6 799.72 28.30 -10 0 -6 842.32 27.80 10 0 6 810.22 27.70 11 0 6 135.49 5.80 -11 0 -6 135.49 5.50 12 0 6 2.90 1.30 -12 0 -6 1.10 1.10 14 -1 -6 30.90 2.10 -14 1 6 33.50 1.70 14 1 -6 34.40 1.80 14 1 -6 37.60 2.30 13 -1 -6 27.30 2.20 13 -1 -6 25.10 1.60 13 1 -6 24.30 2.00 13 1 -6 25.00 1.60 12 -1 -6 5.00 1.30 12 -1 -6 7.80 1.80 12 1 -6 5.10 1.40 12 1 -6 5.70 1.10 12 1 -6 7.30 1.70 11 -1 -6 127.29 4.80 11 -1 -6 108.09 5.00 11 1 -6 112.99 4.60 11 1 -6 107.99 4.90 11 1 -6 109.09 5.10 10 -1 -6 855.41 30.90 10 -1 -6 890.71 30.50 10 -1 -6 940.41 30.60 10 1 -6 926.11 30.60 10 1 -6 911.61 30.40 10 1 -6 894.81 31.00 9 -1 -6 31.50 2.30 9 -1 -6 30.50 2.20 9 -1 -6 31.00 2.10 9 1 -6 31.00 2.00 9 1 -6 33.40 2.40 9 1 -6 30.50 2.10 8 -1 -6 55.69 2.80 8 -1 -6 52.59 3.00 8 -1 -6 53.69 3.00 8 1 -6 59.79 2.80 8 1 -6 60.09 3.10 8 1 -6 59.29 2.90 7 -1 -6 622.54 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4.60 8 -1 6 466.05 16.50 8 -1 6 480.05 16.90 8 1 6 479.45 16.60 -8 1 -6 451.55 16.60 8 1 6 490.55 17.10 9 -1 6 1012.00 34.00 9 -1 6 1007.70 34.80 9 1 6 1031.40 34.10 9 1 6 998.90 34.70 -9 1 -6 992.70 34.10 10 -1 6 11.10 1.90 10 -1 6 8.70 2.30 10 1 6 5.40 1.30 -10 1 -6 9.90 1.70 10 1 6 7.10 1.60 11 -1 6 22.40 3.10 11 1 6 28.60 2.20 -11 1 -6 28.90 2.00 11 1 6 27.50 2.40 12 1 6 125.89 5.40 -12 1 -6 125.39 4.90 -13 1 -6 2.90 0.80 -14 2 6 3.20 0.70 14 2 -6 2.80 0.80 13 -2 -6 -0.30 0.90 -13 2 6 1.60 0.60 13 2 -6 3.00 0.80 13 2 -6 1.30 1.20 12 -2 -6 44.40 2.30 12 -2 -6 41.00 2.60 12 2 -6 37.40 2.10 12 2 -6 35.40 2.50 12 2 -6 38.80 2.00 11 -2 -6 55.99 2.80 11 -2 -6 53.59 3.70 11 2 -6 52.29 3.10 11 2 -6 49.70 2.60 11 2 -6 52.39 2.70 10 -2 -6 26.90 2.10 10 -2 -6 27.60 2.20 10 2 -6 28.80 2.40 10 2 -6 30.00 2.10 10 2 -6 29.10 1.90 9 -2 -6 549.74 18.40 9 -2 -6 512.15 17.90 9 2 -6 480.35 17.80 9 2 -6 502.45 17.90 9 2 -6 535.25 18.30 8 -2 -6 159.08 6.60 8 -2 -6 162.28 6.40 8 2 -6 173.18 6.70 8 2 -6 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3 -6 568.74 19.80 6 3 -6 586.44 19.70 5 -3 -6 77.19 3.50 5 3 -6 74.69 3.40 5 3 -6 77.79 3.50 5 3 -6 70.79 3.80 4 -3 -6 1917.71 62.69 4 3 -6 1861.81 62.59 4 3 -6 1826.02 62.59 -4 3 6 1809.42 63.79 4 3 -6 2015.80 62.59 3 -3 -6 1699.93 55.89 3 -3 -6 1662.33 57.09 3 3 -6 1621.04 55.69 3 3 -6 1696.93 55.69 3 3 -6 1710.23 55.79 2 -3 -6 274.47 11.30 2 -3 -6 286.57 9.90 2 3 -6 264.47 9.90 2 3 -6 271.87 10.00 2 3 -6 271.47 9.80 1 -3 -6 135.69 5.20 1 -3 -6 128.99 6.70 1 3 -6 128.99 5.40 -1 3 6 131.69 5.80 1 3 -6 129.59 5.20 1 3 -6 123.99 5.30 0 -3 -6 59.99 4.30 0 -3 -6 60.39 2.80 0 -3 6 51.19 3.70 0 3 -6 51.79 3.00 0 3 6 52.99 3.20 0 3 -6 56.69 3.30 1 -3 6 23.70 3.10 -1 -3 -6 28.50 5.90 -1 3 -6 20.40 1.90 -1 3 -6 17.00 2.50 1 3 6 22.00 2.30 -1 3 -6 20.60 2.50 1 3 6 25.60 2.30 -1 3 -6 22.80 2.10 2 -3 6 732.33 26.00 2 3 6 709.83 24.30 -2 3 -6 745.43 24.40 -2 3 -6 699.83 24.30 2 3 6 698.23 24.30 -2 3 -6 705.03 24.30 3 3 6 1656.73 55.19 -3 3 -6 1678.23 55.29 -3 3 -6 1574.04 55.09 -3 3 -6 1717.93 55.09 3 3 6 1664.73 55.19 4 3 6 998.10 33.70 4 3 6 1057.89 33.80 4 3 6 1067.29 34.20 -4 3 -6 987.30 33.70 -4 3 -6 892.71 33.60 -4 3 -6 1005.50 33.80 -5 3 -6 215.38 8.30 5 3 6 215.78 8.30 5 3 6 229.18 8.70 5 3 6 220.28 8.30 -5 3 -6 222.78 8.40 6 -3 6 26.00 2.00 -6 3 -6 25.30 2.70 -6 3 -6 26.60 2.20 6 3 6 29.90 2.60 6 3 6 29.30 2.20 7 -3 6 874.81 29.80 -7 3 -6 862.91 30.00 7 3 6 885.91 30.50 7 3 6 895.11 29.90 8 -3 6 112.69 4.70 -8 3 -6 112.59 5.80 8 3 6 105.39 5.20 8 3 6 115.19 4.80 9 -3 6 58.99 2.90 9 3 6 50.49 3.30 9 3 6 54.19 3.00 -9 3 -6 58.49 3.00 10 -3 6 13.00 1.70 -10 3 -6 12.30 1.50 10 3 6 12.10 1.70 10 3 6 11.80 1.60 11 3 6 3.00 1.20 -11 3 -6 1.30 0.70 11 3 6 4.70 1.40 -12 3 -6 3.60 0.90 -13 4 6 3.10 0.70 12 4 -6 24.50 1.80 -12 4 6 22.60 1.30 11 -4 -6 3.60 1.40 11 4 -6 4.70 1.10 -11 4 6 5.60 1.00 11 4 -6 6.80 1.10 10 -4 -6 1.00 1.20 -10 4 6 1.20 0.70 10 4 -6 -0.70 0.70 10 4 -6 0.20 0.70 9 -4 -6 16.20 1.90 -9 4 6 19.30 1.60 9 4 -6 16.70 1.50 9 4 -6 17.60 1.70 8 -4 -6 324.37 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36.40 2.50 9 3 -7 40.10 2.30 9 3 -7 36.70 2.10 8 -3 -7 66.99 4.00 8 3 -7 64.79 3.20 8 3 -7 64.39 3.10 7 -3 -7 423.16 14.70 7 3 -7 394.46 14.30 7 3 -7 407.76 14.40 6 -3 -7 3.90 1.20 6 3 -7 4.10 1.30 6 3 -7 4.10 1.30 5 -3 -7 6.60 1.30 5 3 -7 11.00 2.10 5 3 -7 6.60 1.30 4 -3 -7 142.79 5.70 -4 3 7 128.99 5.90 4 3 -7 144.29 5.70 4 3 -7 138.59 5.50 4 3 -7 150.68 5.80 3 -3 -7 158.78 6.10 3 3 -7 153.48 6.00 3 3 -7 156.58 6.20 3 3 -7 155.68 5.90 -3 3 7 142.39 6.10 2 -3 -7 431.96 14.80 -2 3 7 393.86 14.70 2 3 -7 421.76 14.70 2 3 -7 420.46 14.70 2 3 -7 429.16 14.60 1 -3 -7 51.19 2.70 1 3 -7 47.60 2.70 1 3 -7 53.29 2.80 -1 3 7 47.20 3.10 1 3 -7 49.60 3.00 -1 3 7 50.29 3.90 0 -3 -7 420.56 14.30 0 3 7 413.16 14.10 0 3 7 384.66 14.10 0 3 -7 391.56 14.00 0 3 -7 397.36 14.10 1 3 7 2.00 1.20 -1 3 -7 0.40 1.10 1 3 7 3.60 1.30 -1 3 -7 0.70 0.90 -1 3 -7 -0.60 1.10 -2 3 -7 110.29 4.80 -2 3 -7 109.09 4.80 2 3 7 111.69 4.70 2 3 7 119.19 4.90 -2 3 -7 109.49 4.80 -3 3 -7 12.40 2.40 -3 3 -7 7.80 2.30 -3 3 -7 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14.20 8 4 -7 412.46 14.10 7 -4 -7 338.67 12.50 7 4 -7 343.97 12.20 7 4 -7 345.87 12.20 7 4 -7 350.06 12.30 -7 4 7 337.97 12.10 6 -4 -7 28.30 2.20 6 4 -7 23.60 1.80 6 4 -7 26.90 2.00 6 4 -7 29.10 2.50 -6 4 7 27.30 2.00 5 -4 -7 33.80 2.30 5 4 -7 33.50 2.10 5 4 -7 31.90 2.20 -5 4 7 33.80 2.20 5 4 -7 33.40 2.40 -5 4 7 28.70 3.40 4 -4 -7 315.47 11.00 -4 4 7 286.07 10.70 4 4 -7 294.07 10.80 4 4 -7 290.07 10.80 4 4 -7 302.87 10.80 3 -4 -7 8.10 1.50 3 4 -7 8.90 2.30 -3 4 7 6.90 2.20 3 4 -7 7.10 1.30 3 4 -7 7.10 1.50 3 4 -7 8.80 1.60 2 -4 -7 38.40 2.40 -2 4 7 42.10 2.70 2 4 -7 40.00 2.50 2 4 -7 37.90 2.60 2 4 -7 36.20 2.30 -2 4 7 37.00 3.10 1 -4 -7 427.46 15.10 1 4 -7 422.06 15.00 -1 4 7 423.56 14.90 1 4 -7 427.76 15.00 1 4 -7 415.56 14.80 1 4 -7 422.76 14.80 -1 4 7 426.26 15.00 0 -4 -7 218.98 8.70 0 4 -7 222.08 8.30 0 4 -7 210.88 8.20 0 4 7 213.18 8.30 0 4 7 217.68 8.20 0 4 -7 226.38 8.20 -1 -4 -7 4.70 1.40 1 4 7 3.90 1.50 1 4 7 2.70 1.10 -1 4 -7 2.00 1.00 -1 4 -7 3.90 1.00 -1 4 -7 3.50 1.00 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7 3.60 1.10 -8 6 -7 4.80 0.90 8 6 7 4.20 0.90 6 7 -7 219.88 7.80 6 7 -7 228.08 7.80 5 7 -7 72.79 3.00 5 7 -7 75.29 3.10 4 7 -7 21.70 1.60 4 7 -7 20.40 1.30 3 7 -7 44.50 2.30 3 7 -7 47.10 2.20 -3 7 7 46.20 2.50 -2 7 7 99.39 4.10 2 7 -7 98.99 4.00 2 7 -7 100.69 4.10 1 7 -7 15.20 1.90 -1 7 7 21.30 1.60 1 7 -7 18.90 1.40 -1 7 7 22.30 1.70 1 7 -7 18.00 1.50 0 7 -7 86.79 3.60 0 7 -7 89.89 3.70 0 7 7 87.99 3.60 0 7 7 85.99 3.70 0 7 -7 85.09 3.60 -1 7 -7 27.60 1.70 -1 7 -7 27.70 1.90 1 7 7 27.60 1.90 1 7 7 27.40 1.70 -1 7 -7 25.80 1.60 2 7 7 99.39 4.00 -2 7 -7 100.39 4.00 -2 7 -7 99.29 4.00 2 7 7 103.19 4.60 -2 7 -7 103.39 4.00 3 -7 7 44.80 2.30 3 7 7 49.90 2.40 -3 7 -7 49.50 2.30 -3 7 -7 38.80 2.80 3 7 7 46.30 2.20 -3 7 -7 45.50 2.20 4 -7 7 61.19 2.60 -4 7 -7 60.09 2.60 -4 7 -7 61.99 2.70 4 7 7 62.29 2.70 4 7 7 54.89 2.60 5 -7 7 58.39 2.40 -5 7 -7 52.29 2.90 5 7 7 60.39 2.70 -5 7 -7 58.69 2.40 5 7 7 62.99 2.60 6 -7 7 120.89 4.20 -6 7 -7 107.69 4.20 6 7 7 115.29 4.20 2 8 -7 14.60 1.10 2 8 -7 16.30 1.00 -1 -8 7 19.00 1.20 1 8 -7 19.00 1.20 -1 8 7 19.80 1.50 1 8 -7 17.50 1.10 0 -8 7 24.70 1.30 0 8 -7 24.90 1.40 0 8 7 23.20 1.40 0 8 -7 23.90 1.20 1 -8 7 21.10 1.20 -1 8 -7 24.00 1.20 1 8 7 20.50 1.30 -14 0 8 147.89 5.30 14 0 -8 148.49 5.30 13 0 -8 169.28 6.60 13 0 -8 169.78 6.20 12 0 -8 702.73 23.80 12 0 -8 703.53 24.20 11 0 -8 46.00 2.80 11 0 -8 48.60 2.50 11 0 -8 51.89 2.60 10 0 -8 395.86 15.10 10 0 -8 434.96 14.80 10 0 -8 437.86 14.90 9 0 -8 5.50 1.70 9 0 -8 6.30 1.20 8 0 -8 15.90 1.80 8 0 -8 18.50 1.60 8 0 -8 21.00 1.80 7 0 -8 25.70 1.90 7 0 -8 26.70 2.00 7 0 -8 25.00 2.00 6 0 -8 496.45 17.50 6 0 -8 501.55 17.40 6 0 -8 519.45 17.70 5 0 -8 103.29 4.30 -5 0 8 93.99 5.10 5 0 -8 100.69 4.40 5 0 -8 93.89 4.10 4 0 -8 786.32 27.10 4 0 -8 822.12 27.30 3 0 -8 369.46 13.00 2 0 -8 21.60 1.70 1 0 -8 5750.23 188.88 0 0 -8 9999.00 327.77 -1 0 -8 1356.76 45.30 2 0 8 1.50 1.30 2 0 8 1.40 1.10 3 0 8 903.31 31.00 3 0 8 935.81 31.00 4 0 8 78.59 4.20 4 0 8 88.89 3.80 5 0 8 100.59 4.40 5 0 8 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370.56 13.10 8 3 8 370.76 13.20 -8 3 -8 376.16 13.40 9 -3 8 3.60 0.80 -9 3 -8 4.90 1.20 9 3 8 4.00 1.30 10 -3 8 128.99 5.00 -10 3 -8 133.99 5.20 10 3 8 142.89 5.20 -11 3 -8 289.97 10.20 11 3 8 292.07 10.00 12 4 -8 22.10 1.30 12 4 -8 22.20 1.30 11 -4 -8 17.10 2.10 11 4 -8 17.70 1.20 11 4 -8 19.70 1.20 -11 4 8 16.20 1.20 10 -4 -8 12.30 1.70 10 4 -8 11.50 1.10 -10 4 8 10.40 1.20 10 4 -8 11.20 1.20 9 -4 -8 396.06 14.20 9 4 -8 400.26 14.00 9 4 -8 392.66 13.90 -9 4 8 410.46 13.90 8 -4 -8 34.50 2.40 8 4 -8 36.70 2.20 8 4 -8 32.60 2.00 -8 4 8 36.70 2.10 7 -4 -8 1.30 0.80 7 4 -8 0.60 1.20 7 4 -8 1.00 0.70 -7 4 8 1.40 0.80 7 4 -8 0.60 0.70 6 -4 -8 0.90 0.80 6 4 -8 -0.40 0.80 6 4 -8 0.80 1.10 -6 4 8 1.00 0.90 6 4 -8 0.30 0.70 5 -4 -8 4.90 1.50 5 4 -8 2.00 0.70 5 4 -8 4.10 1.40 5 4 -8 1.70 1.00 -5 4 8 1.20 1.20 -5 4 8 3.50 1.70 4 -4 -8 14.00 1.70 -4 4 8 12.30 2.40 4 4 -8 11.90 1.50 4 4 -8 16.80 2.00 4 4 -8 12.30 1.70 3 -4 -8 399.06 14.00 3 4 -8 390.86 13.80 3 4 -8 377.86 13.80 -3 4 8 376.86 13.70 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1 9 37.10 2.10 11 -1 9 27.60 1.70 11 1 9 29.90 1.70 13 2 -9 2.60 0.70 -13 2 9 2.60 0.70 12 -2 -9 49.00 2.70 12 2 -9 51.79 2.30 12 2 -9 52.59 2.50 -12 2 9 52.19 2.30 11 -2 -9 7.20 1.40 11 -2 -9 10.00 1.90 11 2 -9 8.60 1.20 11 2 -9 9.50 1.00 10 -2 -9 67.99 3.80 10 -2 -9 74.69 3.70 10 2 -9 79.19 3.60 10 2 -9 86.99 3.90 10 2 -9 67.49 3.90 9 -2 -9 36.90 2.50 9 2 -9 40.40 2.30 9 2 -9 40.50 2.20 9 2 -9 36.50 2.90 8 -2 -9 74.59 3.90 8 2 -9 79.69 3.60 8 2 -9 80.29 3.70 7 -2 -9 46.70 2.90 7 2 -9 47.00 2.70 7 2 -9 52.39 3.10 6 -2 -9 175.38 6.90 6 2 -9 163.68 6.60 6 2 -9 169.08 6.50 5 -2 -9 45.10 2.70 5 -2 -9 46.10 2.70 5 2 -9 49.60 2.60 -5 2 9 38.00 3.40 5 2 -9 50.29 2.70 4 -2 -9 60.09 3.10 4 2 -9 57.19 2.90 -4 2 9 55.49 3.30 4 2 -9 58.69 3.00 3 -2 -9 219.98 8.30 3 2 -9 219.08 8.10 -3 2 9 213.18 8.20 3 2 -9 217.38 8.20 3 2 -9 218.28 8.10 2 -2 -9 39.90 2.40 2 2 -9 43.30 2.60 -2 2 9 42.30 2.80 2 2 -9 41.60 2.60 2 2 -9 40.90 2.50 -1 -2 9 3.40 1.50 1 -2 -9 5.50 1.20 -1 2 9 3.20 1.20 1 2 -9 3.50 1.10 1 2 -9 3.40 1.00 1 2 -9 3.50 1.10 -1 2 9 2.30 2.00 0 -2 9 218.48 8.30 0 -2 -9 231.18 8.50 0 2 -9 226.38 8.40 0 2 9 218.88 8.30 0 2 9 228.68 8.40 0 2 -9 223.48 8.30 0 2 -9 205.78 8.30 1 -2 9 36.60 2.50 -1 -2 -9 42.00 2.60 -1 2 -9 42.70 2.70 1 2 9 43.50 2.70 1 2 9 40.90 2.60 2 -2 9 0.80 1.00 -2 2 -9 0.60 1.00 2 2 9 2.10 1.10 2 2 9 1.00 1.00 -3 2 -9 240.38 9.10 3 2 9 259.57 9.60 3 2 9 232.18 9.80 4 -2 9 782.02 26.70 4 2 9 772.52 26.60 -4 2 -9 786.42 26.80 4 2 9 786.12 26.70 5 -2 9 25.40 2.00 5 2 9 29.10 2.60 5 2 9 29.00 2.20 -5 2 -9 26.80 2.30 6 -2 9 235.78 8.90 -6 2 -9 241.78 9.10 6 2 9 241.08 8.90 6 2 9 231.78 9.00 7 -2 9 403.86 14.60 7 2 9 418.76 14.70 -7 2 -9 415.96 14.70 8 -2 9 94.99 4.20 8 2 9 98.99 4.30 -8 2 -9 99.29 4.40 9 -2 9 120.39 4.80 -9 2 -9 122.89 5.00 9 2 9 124.49 5.00 10 -2 9 1.10 0.80 -10 2 -9 1.20 0.80 10 2 9 2.10 0.80 11 2 9 4.60 1.20 12 3 -9 0.30 0.50 -12 3 9 1.00 0.50 12 3 -9 1.10 0.60 11 -3 -9 23.60 1.80 -11 3 9 22.60 1.40 11 3 -9 23.10 1.40 11 3 -9 20.70 1.30 10 -3 -9 28.00 2.00 10 3 -9 22.90 1.50 -10 3 9 25.30 1.60 10 3 -9 25.10 1.60 9 -3 -9 2.30 0.90 9 3 -9 2.90 0.80 9 3 -9 3.30 1.10 8 -3 -9 200.78 8.00 8 3 -9 205.78 7.70 8 3 -9 202.88 7.60 7 -3 -9 27.40 2.20 7 3 -9 26.60 2.00 7 3 -9 30.70 2.00 6 3 -9 18.70 1.70 6 3 -9 23.70 2.30 6 3 -9 18.20 1.80 5 -3 -9 121.49 5.20 5 3 -9 114.89 5.00 5 3 -9 115.69 5.00 5 3 -9 120.59 5.20 -5 3 9 121.59 5.20 4 -3 -9 191.38 7.50 -4 3 9 182.18 7.30 4 3 -9 196.38 7.30 4 3 -9 185.48 7.10 4 3 -9 181.98 7.20 3 -3 -9 2.00 0.80 3 3 -9 0.00 1.00 3 3 -9 0.50 0.80 3 3 -9 0.90 0.70 -3 3 9 3.10 1.20 2 -3 -9 27.00 2.00 2 3 -9 30.40 2.40 2 3 -9 28.40 2.10 2 3 -9 25.40 2.20 1 -3 -9 6.90 1.30 1 3 -9 3.80 1.20 1 3 -9 4.80 1.10 -1 3 9 7.10 1.90 1 3 -9 7.40 2.30 0 -3 -9 139.29 5.80 0 3 9 131.89 5.60 0 3 -9 134.59 5.80 0 3 -9 134.79 5.70 0 3 -9 135.69 5.50 0 3 9 132.89 5.70 -1 -3 -9 72.69 3.60 1 -3 9 72.09 3.50 -1 3 -9 71.09 3.50 -1 3 -9 67.89 3.50 -1 3 -9 66.89 3.50 1 3 9 69.29 3.60 -2 -3 -9 551.34 18.50 2 -3 9 520.05 18.10 -2 3 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-7 4 9 13.70 1.90 6 -4 -9 96.19 4.60 6 4 -9 112.89 4.60 6 4 -9 112.29 4.60 -6 4 9 107.59 4.50 6 4 -9 103.59 4.50 5 -4 -9 236.18 9.20 5 4 -9 243.88 8.90 5 4 -9 243.48 9.00 -5 4 9 239.68 9.10 5 4 -9 247.18 9.00 4 -4 -9 192.18 7.80 4 4 -9 199.58 7.60 -4 4 9 204.48 7.70 4 4 -9 189.48 7.40 4 4 -9 202.38 7.60 3 4 -9 382.16 13.90 3 4 -9 391.46 13.80 3 4 -9 391.56 14.00 -3 4 9 401.16 14.00 2 4 -9 91.39 4.00 -2 4 9 87.79 4.20 2 4 -9 85.69 4.10 2 4 -9 85.99 4.10 1 -4 -9 37.90 2.50 -1 4 9 36.20 2.50 1 4 -9 34.90 2.30 1 4 -9 34.90 2.30 1 4 -9 34.10 2.80 -1 4 9 32.30 2.70 0 -4 -9 144.49 6.00 0 4 9 138.29 5.80 0 4 -9 141.39 5.80 0 4 -9 141.79 5.90 0 4 -9 142.29 5.70 0 4 9 138.99 5.90 -1 -4 -9 497.55 18.20 1 4 9 497.45 17.50 -1 4 -9 500.05 17.40 -1 4 -9 497.55 17.50 -1 4 -9 493.05 17.30 1 4 9 496.15 17.40 2 -4 9 269.67 10.10 -2 -4 -9 271.27 10.20 2 4 9 261.37 9.90 -2 4 -9 267.57 9.80 -2 4 -9 268.17 9.80 2 4 9 262.07 9.90 -3 -4 -9 278.77 10.80 3 -4 9 277.47 10.40 3 4 9 285.37 10.60 3 4 9 288.87 10.50 -3 4 -9 288.27 10.30 -3 4 -9 284.97 10.60 4 -4 9 40.60 2.40 -4 -4 -9 37.50 2.70 -4 4 -9 40.40 2.50 4 4 9 41.50 2.80 -4 4 -9 33.30 2.70 4 4 9 36.80 2.50 5 -4 9 91.29 4.10 -5 4 -9 95.19 4.30 5 4 9 99.09 4.40 5 4 9 96.69 4.30 -6 4 -9 404.86 15.10 6 4 9 390.26 13.90 6 4 9 392.06 15.30 7 -4 9 434.56 15.20 7 4 9 439.36 15.40 -7 4 -9 445.96 15.40 8 -4 9 92.59 3.70 -8 4 -9 90.49 3.90 8 4 9 94.49 3.90 -9 -4 -9 11.30 1.60 9 -4 9 10.00 1.10 -9 4 -9 11.30 1.10 9 4 9 10.60 1.10 -10 4 -9 42.20 1.80 10 4 9 37.60 2.00 10 5 -9 0.60 0.50 10 5 -9 1.20 0.50 -10 5 9 2.60 0.90 9 5 -9 27.50 1.50 -9 5 9 25.90 1.60 9 5 -9 27.20 1.50 8 -5 -9 8.80 2.00 -8 5 9 9.90 1.40 8 5 -9 11.60 1.00 8 5 -9 11.00 1.20 7 -5 -9 10.30 1.80 7 5 -9 13.00 1.20 7 5 -9 11.70 1.20 -7 5 9 6.90 2.00 6 -5 -9 -0.20 1.00 6 5 -9 1.20 0.90 6 5 -9 1.40 0.70 6 5 -9 1.00 0.60 5 -5 -9 158.08 6.60 5 5 -9 170.18 6.40 5 5 -9 180.38 7.40 -5 5 9 164.38 6.70 4 -5 -9 219.38 9.00 4 5 -9 239.88 8.90 4 5 -9 250.27 8.90 -4 5 9 246.38 8.90 4 5 -9 235.38 8.70 3 -5 -9 18.30 1.90 3 5 -9 18.30 1.80 -3 5 9 25.30 2.20 3 5 -9 19.60 1.70 3 5 -9 22.80 2.00 2 -5 -9 253.97 10.10 2 5 -9 284.47 10.30 2 5 -9 273.57 10.00 2 5 -9 270.67 9.90 -2 5 9 278.37 10.10 1 -5 -9 130.59 5.70 1 5 -9 138.09 5.50 -1 5 9 137.89 5.60 -1 5 9 131.39 6.80 1 5 -9 133.69 5.60 1 5 -9 136.09 6.30 0 -5 -9 90.59 4.40 0 5 -9 97.19 4.10 0 5 9 92.19 4.20 0 5 -9 94.69 4.30 0 5 -9 94.19 4.30 0 5 9 95.39 4.30 -1 -5 -9 48.80 3.00 -1 5 -9 52.89 3.00 1 5 9 51.89 3.00 -1 5 -9 55.29 2.90 -1 5 -9 56.29 2.90 1 5 9 53.19 2.90 -2 -5 -9 5.90 1.60 2 5 9 3.80 1.20 2 5 9 5.90 1.60 -2 5 -9 9.10 1.60 -2 5 -9 5.40 1.40 -2 5 -9 9.00 1.60 3 -5 9 45.90 2.50 -3 -5 -9 40.90 2.80 -3 5 -9 46.50 2.60 3 5 9 48.10 2.70 3 5 9 43.30 2.70 -3 5 -9 45.60 3.60 4 -5 9 13.80 1.50 -4 -5 -9 17.20 1.90 4 5 9 17.10 1.90 -4 5 -9 16.60 1.60 4 5 9 17.90 1.60 -4 5 -9 15.60 1.70 -5 -5 -9 62.49 3.20 5 -5 9 58.29 2.80 5 5 9 57.99 2.90 -5 5 -9 61.99 3.00 -5 5 -9 56.59 2.90 5 5 9 60.69 3.00 -6 -5 -9 28.40 2.20 6 -5 9 28.20 1.70 6 5 9 29.50 1.80 -6 5 -9 27.10 1.80 6 5 9 28.80 2.00 -7 -5 -9 23.60 2.00 7 -5 9 23.00 1.40 7 5 9 23.00 1.50 -7 5 -9 21.60 1.60 8 -5 9 2.60 0.80 8 5 9 2.70 0.90 -8 5 -9 2.20 0.80 8 6 -9 0.40 0.50 7 6 -9 21.00 1.40 7 6 -9 20.60 1.20 6 6 -9 8.50 1.00 6 6 -9 10.10 1.10 5 6 -9 13.70 1.20 5 6 -9 14.90 1.30 5 6 -9 13.00 1.40 4 6 -9 128.19 4.90 -4 6 9 125.09 5.00 4 6 -9 122.59 4.90 4 6 -9 124.09 5.00 3 -6 -9 21.90 2.50 -3 6 9 21.70 2.00 3 6 -9 23.50 1.70 3 6 -9 23.60 1.60 3 6 -9 27.70 2.30 2 -6 -9 33.50 2.70 2 6 -9 31.30 1.90 -2 6 9 32.80 2.20 2 6 -9 29.80 2.00 2 6 -9 32.10 1.90 1 -6 -9 93.29 4.50 1 6 -9 96.59 4.10 -1 6 9 99.59 4.20 -1 6 9 95.19 4.10 1 6 -9 96.09 4.00 1 6 -9 93.49 4.00 0 -6 -9 198.98 7.90 0 6 9 193.18 7.30 0 6 9 199.88 7.50 0 6 -9 200.78 7.40 0 6 -9 200.68 7.40 0 6 -9 200.48 7.40 -1 -6 -9 639.94 21.50 1 -6 9 619.14 21.20 -1 6 -9 626.24 21.20 1 6 9 621.34 21.10 1 6 9 597.54 21.20 -1 6 -9 616.14 21.10 -1 6 -9 625.44 21.10 2 -6 9 38.70 2.10 -2 -6 -9 40.90 2.70 -2 6 -9 36.10 2.10 2 6 9 42.00 2.30 -2 6 -9 39.20 2.10 2 6 9 37.70 2.10 -3 -6 -9 54.39 3.00 3 -6 9 51.49 2.40 -3 6 -9 49.40 2.50 -3 6 -9 50.79 2.40 3 6 9 52.19 2.60 3 6 9 49.60 2.50 -4 -6 -9 227.68 8.70 4 -6 9 242.38 8.50 4 6 9 234.38 8.40 -4 6 -9 232.58 8.40 4 6 9 225.78 8.30 -4 6 -9 233.68 8.20 5 -6 9 69.79 3.00 -5 6 -9 61.59 2.70 -5 6 -9 66.89 2.80 5 6 9 61.39 2.80 5 6 9 62.59 3.30 6 -6 9 108.39 3.90 6 6 9 104.59 4.10 -6 6 -9 101.69 4.00 7 -6 9 54.29 2.30 -7 6 -9 61.69 2.40 7 6 9 58.79 2.30 5 7 -9 22.00 1.20 4 7 -9 120.19 4.40 3 7 -9 3.40 0.80 -3 7 9 2.40 1.00 3 7 -9 1.50 0.60 -2 -7 9 14.20 1.40 -2 7 9 16.50 1.40 2 7 -9 14.80 1.00 2 7 -9 11.10 1.10 2 7 -9 11.60 1.40 -1 -7 9 4.80 1.00 -1 7 9 5.50 1.20 1 7 -9 3.20 0.90 1 7 -9 2.30 0.80 0 -7 9 8.90 1.20 0 7 -9 9.00 1.20 0 7 -9 9.00 0.90 0 7 9 11.10 1.20 1 -7 9 106.29 4.30 -1 7 -9 106.99 4.20 1 7 9 111.49 4.40 1 7 9 101.29 4.00 -1 7 -9 107.89 4.00 2 -7 9 255.77 8.60 2 7 9 235.38 8.70 -2 7 -9 248.78 8.60 2 7 9 253.97 8.60 -2 7 -9 249.97 8.60 3 -7 9 37.80 1.70 3 7 9 33.40 1.70 3 7 9 37.00 1.80 -3 7 -9 37.40 1.70 13 0 -10 15.40 1.10 12 0 -10 4.00 1.10 12 0 -10 4.00 0.90 11 0 -10 149.79 5.70 11 0 -10 153.58 5.70 10 0 -10 20.70 1.60 10 0 -10 17.00 1.80 10 0 -10 15.80 2.20 9 0 -10 258.87 10.20 9 0 -10 277.77 9.90 9 0 -10 280.57 9.90 8 0 -10 778.82 26.00 8 0 -10 762.82 26.00 8 0 -10 759.02 26.50 7 0 -10 26.80 2.00 7 0 -10 31.70 2.90 7 0 -10 29.00 2.20 6 0 -10 310.57 11.10 6 0 -10 303.77 10.70 -6 0 10 286.47 10.90 6 0 -10 284.87 10.70 -5 0 10 238.18 9.20 5 0 -10 244.28 9.10 5 0 -10 238.28 8.90 4 0 -10 60.39 3.10 4 0 -10 57.49 3.30 -4 0 10 58.09 3.20 4 0 -10 59.49 3.10 3 0 -10 17.00 1.70 3 0 -10 17.50 2.40 -3 0 10 19.60 2.10 3 0 -10 15.10 2.50 -2 0 10 753.42 26.30 2 0 -10 795.02 26.50 -1 0 10 562.44 20.10 1 0 -10 607.64 20.30 0 0 10 3.60 1.40 0 0 -10 2.30 0.90 0 0 10 1.30 1.00 1 0 10 11.70 1.90 1 0 10 6.60 1.80 -1 0 -10 9.30 1.70 -2 0 -10 7.10 1.70 2 0 10 5.80 1.60 2 0 10 6.50 1.70 3 0 10 14.80 2.10 -3 0 -10 11.70 1.80 3 0 10 12.70 1.60 4 0 10 311.87 11.10 4 0 10 297.17 11.10 5 0 10 46.30 3.10 5 0 10 42.00 2.60 6 0 10 44.50 2.60 7 0 10 293.37 10.70 8 0 10 767.52 27.50 9 0 10 0.10 0.70 10 0 10 242.38 8.60 11 0 10 347.97 11.80 13 1 -10 42.60 1.80 -13 1 10 40.40 1.80 12 -1 -10 26.60 1.90 12 -1 -10 28.20 1.70 12 1 -10 28.30 1.50 11 -1 -10 7.60 1.30 11 -1 -10 6.70 1.70 11 1 -10 6.80 0.90 11 1 -10 6.20 1.00 11 1 -10 6.40 1.80 10 -1 -10 81.89 3.60 10 -1 -10 72.19 3.80 10 1 -10 83.29 3.50 10 1 -10 84.59 3.60 10 1 -10 93.79 4.00 9 -1 -10 21.00 2.00 9 -1 -10 17.00 1.80 9 -1 -10 21.80 1.60 9 1 -10 17.20 1.50 9 1 -10 20.20 1.70 9 1 -10 18.50 2.00 8 -1 -10 95.29 4.60 8 -1 -10 98.79 4.40 8 -1 -10 108.09 4.40 8 1 -10 103.89 4.70 8 1 -10 103.59 4.40 8 1 -10 106.69 4.30 7 -1 -10 357.26 12.00 7 -1 -10 321.77 12.30 7 -1 -10 318.87 12.00 7 1 -10 335.07 11.90 7 1 -10 337.97 12.00 7 1 -10 343.87 12.50 6 -1 -10 180.58 7.00 -6 -1 10 167.38 6.90 6 -1 -10 178.58 6.60 6 1 -10 169.48 6.60 6 1 -10 172.58 6.80 6 1 -10 174.08 6.90 -6 1 10 163.58 7.10 5 -1 -10 20.50 1.90 5 -1 -10 20.20 3.00 5 1 -10 19.00 1.90 5 1 -10 18.10 1.70 5 1 -10 20.10 2.10 4 -1 -10 5.70 1.30 4 -1 -10 4.00 1.40 4 1 -10 5.30 1.10 4 1 -10 6.20 1.70 4 1 -10 6.00 1.70 -4 1 10 5.30 1.30 3 -1 -10 145.69 5.70 3 1 -10 122.19 5.50 -3 1 10 131.59 5.50 3 1 -10 136.49 5.50 3 1 -10 135.09 5.50 2 -1 -10 4.00 1.30 2 1 -10 5.50 1.20 2 1 -10 5.10 1.50 -2 1 10 4.00 1.20 1 -1 -10 268.67 9.60 -1 -1 10 242.98 9.40 1 1 -10 254.07 9.40 -1 1 10 254.57 9.40 0 -1 -10 906.71 29.90 0 -1 10 863.31 29.60 0 1 10 867.31 29.60 0 1 -10 870.81 29.70 0 1 10 878.41 29.70 -1 -1 -10 71.69 3.50 1 -1 10 70.09 3.40 1 1 10 67.99 3.50 1 1 10 70.49 3.50 -1 1 -10 69.09 3.70 -2 -1 -10 21.60 2.00 2 -1 10 16.60 1.90 -2 1 -10 18.50 2.40 2 1 10 23.70 2.00 3 -1 10 93.99 4.60 3 -1 10 91.89 4.30 -3 -1 -10 98.49 4.50 3 1 10 94.69 4.30 3 1 10 99.39 4.40 4 -1 10 8.70 1.90 4 -1 10 5.20 1.40 -4 1 -10 6.40 1.50 4 1 10 3.60 1.10 4 1 10 7.20 2.00 5 -1 10 116.09 4.90 5 -1 10 110.09 4.80 5 1 10 109.29 4.90 5 1 10 106.89 5.00 -5 1 -10 111.39 5.00 6 -1 10 152.68 6.20 -6 1 -10 156.28 6.30 6 1 10 153.98 6.30 7 -1 10 197.58 7.50 7 1 10 197.18 7.50 -7 1 -10 192.78 7.60 8 -1 10 0.80 0.80 -8 1 -10 -0.40 1.30 8 1 10 0.00 0.70 9 -1 10 57.19 2.80 9 1 10 62.09 2.80 -9 1 -10 59.09 3.20 10 -1 10 76.09 3.30 10 1 10 89.89 3.40 13 2 -10 60.09 2.40 -13 2 10 59.39 2.30 12 -2 -10 12.30 1.50 12 2 -10 10.90 0.90 12 2 -10 11.70 1.10 -12 2 10 10.00 0.90 11 -2 -10 0.60 0.90 11 2 -10 0.10 0.40 11 2 -10 0.70 0.50 10 -2 -10 11.60 1.50 10 2 -10 12.50 1.30 10 2 -10 9.60 1.20 9 -2 -10 101.49 5.00 9 2 -10 114.79 4.70 9 2 -10 116.99 4.60 8 -2 -10 111.99 5.60 8 2 -10 131.79 5.10 8 2 -10 129.79 5.20 7 -2 -10 17.00 1.80 7 2 -10 20.70 1.60 7 2 -10 20.00 1.70 6 2 -10 212.98 8.10 6 2 -10 213.68 8.00 5 -2 -10 39.70 2.60 5 2 -10 38.70 2.50 5 2 -10 48.40 2.50 -5 2 10 36.20 3.10 4 -2 -10 22.00 1.90 4 2 -10 25.20 2.00 4 2 -10 21.80 1.90 -4 2 10 22.40 2.50 3 -2 -10 3.90 1.00 -3 2 10 6.00 1.90 3 2 -10 4.80 1.50 3 2 -10 3.90 1.00 2 -2 -10 53.29 3.00 2 2 -10 53.29 3.00 -2 2 10 53.19 3.70 -1 -2 10 273.77 10.50 1 -2 -10 303.97 10.90 1 2 -10 306.67 10.90 1 2 -10 289.77 10.50 -1 2 10 289.27 12.00 0 -2 -10 610.94 20.20 0 -2 10 584.74 19.90 0 2 10 589.14 19.90 0 2 -10 562.94 20.00 0 2 -10 508.95 20.50 0 2 10 595.44 20.00 1 -2 10 2.60 0.90 -1 -2 -10 4.50 1.40 -1 2 -10 5.40 1.70 1 2 10 3.50 1.10 -2 -2 -10 10.60 1.70 2 -2 10 12.00 1.60 2 2 10 8.20 1.70 2 2 10 9.30 1.80 -2 2 -10 11.70 1.90 3 -2 10 122.79 5.20 -3 -2 -10 126.99 5.50 3 2 10 119.59 5.20 -3 2 -10 122.39 5.30 3 2 10 126.69 5.20 4 -2 10 132.99 5.50 4 -2 10 128.59 5.50 -4 2 -10 132.19 5.60 4 2 10 136.59 5.50 4 2 10 132.79 5.60 5 -2 10 203.58 7.90 5 -2 10 210.58 8.00 5 2 10 215.58 8.00 -5 2 -10 216.58 8.10 5 2 10 201.78 8.00 6 -2 10 14.00 1.60 6 2 10 13.80 2.30 -6 2 -10 15.90 2.00 6 2 10 13.90 1.70 7 -2 10 72.29 3.40 -7 2 -10 72.99 3.70 7 2 10 71.19 3.50 8 -2 10 313.67 11.20 8 2 10 306.67 11.20 -8 2 -10 325.47 11.30 9 -2 10 24.60 1.60 9 2 10 22.30 1.60 -9 2 -10 26.70 1.80 10 -2 10 6.50 1.00 10 2 10 4.40 1.20 -10 2 -10 7.10 1.50 12 3 -10 0.10 0.40 -12 3 10 0.60 0.50 12 3 -10 -0.30 0.40 11 -3 -10 27.20 1.90 11 3 -10 29.70 1.60 11 3 -10 27.70 1.50 -11 3 10 29.70 1.50 10 -3 -10 21.20 1.70 10 3 -10 21.40 1.40 -10 3 10 20.50 1.40 10 3 -10 19.40 1.30 9 -3 -10 197.58 7.80 9 3 -10 198.08 7.40 9 3 -10 196.68 7.30 -9 3 10 201.48 7.20 8 -3 -10 371.86 14.30 8 3 -10 418.96 14.00 8 3 -10 421.26 14.10 -8 3 10 385.66 13.80 7 -3 -10 466.65 17.90 7 3 -10 531.65 17.70 7 3 -10 522.25 17.60 6 -3 -10 77.89 3.80 6 3 -10 74.39 3.60 6 3 -10 73.99 3.60 5 -3 -10 85.49 4.30 5 3 -10 93.69 4.10 -5 3 10 94.69 4.40 5 3 -10 91.19 4.00 4 -3 -10 860.91 30.20 4 3 -10 817.62 28.00 4 3 -10 806.52 28.10 -4 3 10 820.82 28.10 4 3 -10 822.22 28.00 3 -3 -10 683.93 23.30 3 3 -10 669.03 23.00 3 3 -10 665.33 22.80 -3 3 10 669.63 22.90 3 3 -10 649.04 22.90 2 -3 -10 279.97 10.30 -2 -3 10 253.97 10.00 -2 3 10 277.57 10.10 2 3 -10 272.27 10.10 2 3 -10 271.17 10.20 2 3 -10 280.57 10.00 -1 -3 10 457.75 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9.90 2 1 13 266.17 9.70 2 1 13 274.17 9.80 -3 -1 -13 17.80 2.00 3 -1 13 15.70 1.90 3 -1 13 18.20 2.10 3 1 13 19.00 2.40 4 -1 13 16.90 1.60 4 -1 13 15.10 1.90 -4 -1 -13 13.80 2.00 4 1 13 16.70 1.60 4 1 13 14.70 1.80 -5 -1 -13 153.88 6.30 5 -1 13 156.98 6.00 5 -1 13 157.78 5.90 5 1 13 159.08 6.10 5 1 13 155.88 6.00 6 -1 13 76.69 3.20 6 1 13 68.79 3.10 7 -1 13 27.60 1.60 7 1 13 29.20 1.60 8 -1 13 42.20 1.90 8 1 13 41.00 1.90 10 2 -13 10.70 1.00 10 2 -13 10.30 0.90 9 -2 -13 37.80 2.20 9 2 -13 38.60 1.80 9 2 -13 36.30 1.80 8 -2 -13 43.70 2.60 8 2 -13 48.70 2.30 8 2 -13 48.90 2.20 7 -2 -13 181.48 7.00 -7 -2 13 164.18 6.60 7 2 -13 182.38 6.50 7 2 -13 178.48 6.60 -6 -2 13 3.60 1.10 6 -2 -13 6.50 1.40 6 2 -13 4.90 1.10 -6 2 13 4.20 1.40 6 2 -13 7.20 1.20 -5 -2 13 2.10 0.90 5 -2 -13 4.10 1.30 5 2 -13 2.50 0.80 -5 2 13 3.10 1.10 5 2 -13 2.50 0.80 4 -2 -13 12.50 1.60 -4 -2 13 14.20 1.80 4 2 -13 15.30 2.30 -4 2 13 16.10 3.30 4 2 -13 14.20 1.70 3 -2 -13 362.26 14.30 -3 -2 13 413.26 14.20 3 2 -13 396.06 14.30 3 2 -13 418.66 14.10 -3 2 13 413.26 14.20 2 -2 -13 6.90 1.50 -2 2 13 7.70 2.20 2 2 -13 8.30 1.60 -1 -2 13 0.10 0.90 1 -2 -13 0.50 0.90 -1 2 13 -1.00 0.90 1 2 -13 1.10 0.90 0 -2 -13 15.30 1.80 0 -2 13 16.90 2.00 0 -2 13 14.90 1.80 0 2 13 15.50 1.90 0 2 -13 17.40 1.90 1 -2 13 28.60 2.30 1 -2 13 31.30 2.20 -1 -2 -13 28.60 2.20 1 2 13 28.00 2.20 -1 2 -13 29.90 2.50 2 -2 13 0.80 1.00 -2 -2 -13 0.30 0.90 2 -2 13 1.40 0.90 -2 2 -13 0.50 0.90 2 2 13 1.80 1.00 3 -2 13 285.37 10.50 3 -2 13 297.17 10.50 -3 -2 -13 279.97 10.80 3 2 13 299.47 10.60 -3 2 -13 301.97 10.60 3 2 13 296.17 10.60 4 -2 13 124.49 5.00 4 -2 13 130.39 5.10 -4 -2 -13 125.29 5.40 4 2 13 131.39 5.10 -4 2 -13 128.09 5.10 4 2 13 127.89 5.10 5 -2 13 21.90 1.70 -5 -2 -13 24.10 2.00 5 2 13 24.30 1.80 5 2 13 24.00 1.60 -5 2 -13 28.60 2.10 6 -2 13 234.98 8.50 -6 -2 -13 235.28 8.70 6 2 13 239.48 8.50 7 -2 13 69.39 2.90 7 2 13 73.69 3.00 8 -2 13 84.39 3.30 8 2 13 90.09 3.30 9 3 -13 47.20 2.00 9 3 -13 44.90 1.90 8 -3 -13 47.50 2.50 8 3 -13 45.00 2.10 8 3 -13 48.50 2.20 -7 -3 13 2.50 1.80 7 -3 -13 3.10 1.00 7 3 -13 3.30 0.90 7 3 -13 3.70 0.90 6 -3 -13 9.10 1.30 -6 -3 13 9.50 1.50 6 3 -13 8.50 1.10 6 3 -13 9.20 1.10 5 -3 -13 216.98 8.50 -5 -3 13 228.88 8.30 5 3 -13 232.18 8.30 -5 3 13 226.88 8.30 5 3 -13 228.18 8.10 4 -3 -13 10.10 1.60 -4 3 13 11.10 1.60 4 3 -13 8.50 1.30 4 3 -13 12.20 1.30 3 -3 -13 1.10 0.80 3 3 -13 1.70 0.70 3 3 -13 4.60 1.40 -3 3 13 2.50 0.90 2 -3 -13 11.00 1.50 -2 3 13 11.40 1.70 2 3 -13 11.00 1.80 2 3 -13 10.10 1.40 1 -3 -13 0.90 0.90 1 3 -13 0.10 0.80 -1 3 13 1.80 0.90 0 -3 13 14.20 1.80 0 -3 -13 16.50 1.80 0 3 -13 15.50 1.60 0 3 13 17.80 1.80 1 -3 13 68.29 3.20 -1 -3 -13 72.19 4.10 1 -3 13 69.89 3.20 1 3 13 65.49 3.20 1 3 13 64.29 3.20 -1 3 -13 67.89 3.20 2 -3 13 26.90 1.90 2 -3 13 27.20 1.80 -2 -3 -13 28.10 2.10 -2 3 -13 29.80 1.90 2 3 13 25.00 1.90 2 3 13 28.30 1.90 -3 -3 -13 15.00 1.80 3 -3 13 14.20 1.50 3 -3 13 14.60 1.40 3 3 13 16.50 1.50 -3 3 -13 14.00 1.40 3 3 13 14.40 1.50 -4 -3 -13 1.00 0.90 4 -3 13 1.40 0.70 4 -3 13 -1.00 0.90 4 3 13 0.70 0.80 -4 3 -13 1.00 0.70 4 3 13 0.30 0.80 -5 -3 -13 1.20 1.00 5 -3 13 2.00 0.60 5 3 13 0.70 0.60 -5 3 -13 1.60 0.80 6 -3 13 7.90 0.90 -6 3 -13 6.60 1.20 6 3 13 5.20 0.90 7 -3 13 38.60 1.70 7 3 13 39.20 1.80 8 4 -13 3.30 0.70 8 4 -13 1.60 0.50 7 4 -13 2.20 0.70 7 4 -13 1.80 0.50 6 -4 -13 54.59 2.80 6 4 -13 58.99 2.40 6 4 -13 58.89 2.50 -5 -4 13 105.59 4.20 5 -4 -13 105.79 4.50 5 4 -13 104.29 4.10 5 4 -13 107.99 4.20 4 -4 -13 233.68 8.90 4 4 -13 246.38 8.50 -4 4 13 239.68 8.60 4 4 -13 244.18 8.70 3 -4 -13 104.59 4.60 3 4 -13 107.29 4.30 3 4 -13 110.19 4.20 -3 4 13 108.19 4.40 2 -4 -13 17.00 1.70 2 4 -13 17.20 1.40 2 4 -13 17.70 1.60 -2 4 13 17.50 1.60 1 4 -13 36.20 2.20 1 4 -13 35.80 2.00 -1 4 13 38.60 2.20 0 -4 -13 83.39 3.90 0 -4 13 80.89 3.50 0 4 13 84.59 3.80 0 4 -13 83.09 3.60 -1 -4 -13 65.89 3.20 1 -4 13 66.29 2.90 1 -4 13 67.09 3.00 1 4 13 64.19 3.00 1 4 13 62.89 3.20 -1 4 -13 63.99 3.00 2 -4 13 67.69 2.90 2 -4 13 67.99 2.90 -2 -4 -13 68.19 3.30 -2 4 -13 67.09 3.00 2 4 13 67.89 3.30 2 4 13 66.09 3.00 3 -4 13 129.59 4.90 3 -4 13 119.39 5.40 -3 -4 -13 133.89 5.30 -3 4 -13 131.49 5.00 3 4 13 130.49 4.90 3 4 13 132.89 5.00 4 -4 13 94.09 3.60 -4 -4 -13 94.99 4.00 -4 4 -13 96.89 3.70 4 4 13 89.99 3.90 4 4 13 89.89 4.10 5 -4 13 21.30 1.20 5 4 13 18.60 1.30 -5 4 -13 20.50 1.30 6 5 -13 0.70 0.50 6 5 -13 1.10 0.50 -5 -5 13 109.99 4.10 5 5 -13 113.19 4.10 5 5 -13 110.39 4.10 4 5 -13 71.89 3.30 4 5 -13 88.49 3.10 3 5 -13 15.60 1.20 3 5 -13 16.90 1.20 -3 5 13 17.80 1.50 2 -5 -13 79.59 3.60 2 5 -13 79.89 3.20 2 5 -13 78.89 3.10 -2 5 13 79.29 3.50 1 -5 -13 82.09 3.70 1 5 -13 86.59 3.40 1 5 -13 79.89 3.30 -1 5 13 85.19 3.40 0 -5 13 11.80 1.20 0 -5 -13 10.30 1.60 0 5 -13 11.70 1.00 0 5 13 13.50 1.70 1 -5 13 10.50 1.20 1 -5 13 11.80 1.30 -1 5 -13 13.90 1.10 1 5 13 11.50 1.20 2 -5 13 -0.20 0.70 2 -5 13 -0.20 0.80 2 5 13 0.10 0.60 -2 5 -13 0.40 0.40 3 -5 13 4.60 0.90 -3 5 -13 4.50 0.80 3 5 13 2.70 0.70 -6 0 14 110.59 4.50 -5 0 14 262.07 9.50 -4 0 14 224.18 8.30 -3 0 14 19.30 2.00 -2 0 14 70.29 4.00 -1 0 14 44.20 2.70 1 0 14 22.50 2.10 1 0 14 21.10 1.80 2 0 14 26.30 2.00 2 0 14 27.70 2.00 3 0 14 2.10 0.80 3 0 14 2.50 0.90 4 0 14 98.39 4.00 4 0 14 92.09 4.00 5 0 14 28.70 2.20 5 0 14 30.40 1.80 6 0 14 1.70 0.60 7 0 14 153.18 5.50 8 -1 -14 29.30 2.40 8 1 -14 37.10 2.00 8 1 -14 34.30 2.00 7 -1 -14 100.39 4.40 7 1 -14 102.39 4.10 7 1 -14 105.09 4.00 6 -1 -14 98.19 4.20 -6 -1 14 93.19 3.90 -6 1 14 88.39 4.10 6 1 -14 94.59 3.90 6 1 -14 94.99 3.90 5 -1 -14 14.60 2.20 -5 -1 14 18.00 1.70 -5 1 14 16.00 1.90 5 1 -14 18.10 1.80 4 -1 -14 85.59 4.00 -4 -1 14 88.99 3.90 -4 1 14 87.89 3.90 4 1 -14 87.79 3.90 3 -1 -14 12.30 1.80 -3 -1 14 14.60 1.70 -3 1 14 13.30 1.80 3 1 -14 11.40 2.10 -2 -1 14 36.90 2.90 2 -1 -14 37.30 2.50 -2 1 14 43.80 2.80 -1 -1 14 59.79 4.00 1 -1 -14 56.39 3.10 -1 1 14 56.09 3.70 0 -1 -14 211.48 8.30 0 -1 14 217.98 8.20 0 1 14 223.28 8.20 -1 -1 -14 44.10 2.80 1 -1 14 46.90 2.60 1 -1 14 51.39 2.60 1 1 14 50.79 2.70 1 1 14 44.50 2.80 -2 -1 -14 13.70 2.10 2 -1 14 14.40 1.60 2 -1 14 15.50 1.60 2 1 14 12.50 1.60 2 1 14 12.60 1.70 3 -1 14 6.10 1.40 3 -1 14 7.90 1.30 -3 -1 -14 9.50 2.30 3 1 14 9.80 1.40 3 1 14 7.80 1.50 4 -1 14 -0.20 0.70 4 -1 14 1.00 0.80 4 1 14 0.20 0.80 4 1 14 0.70 0.80 5 -1 14 79.59 3.20 5 1 14 73.19 3.20 5 1 14 73.19 3.10 6 -1 14 63.29 2.70 6 1 14 63.49 2.70 7 -1 14 27.70 1.40 7 1 14 29.50 1.50 9 2 -14 14.10 1.10 9 2 -14 13.60 1.20 8 2 -14 24.10 1.40 8 2 -14 23.20 1.40 7 -2 -14 26.70 2.00 7 2 -14 26.10 1.60 7 2 -14 28.60 1.50 6 -2 -14 277.67 10.10 -6 -2 14 269.27 9.70 6 2 -14 287.77 9.80 6 2 -14 276.87 9.60 5 -2 -14 0.20 0.90 -5 -2 14 0.70 0.90 5 2 -14 1.50 0.90 -5 2 14 1.90 1.10 5 2 -14 1.90 0.70 -4 -2 14 2.60 0.80 -4 2 14 2.00 0.90 4 2 -14 4.10 1.20 3 -2 -14 1.00 1.00 -3 -2 14 0.30 0.70 -3 2 14 1.30 0.80 3 2 -14 1.90 0.90 2 -2 -14 73.29 3.60 -2 -2 14 73.09 3.40 2 2 -14 75.19 3.40 -2 2 14 79.39 3.60 1 -2 -14 22.30 2.00 -1 -2 14 25.50 1.90 -1 2 14 27.90 2.00 1 2 -14 26.70 1.90 0 -2 -14 122.39 5.30 0 -2 14 130.19 5.20 0 2 -14 124.79 5.00 0 2 14 128.69 5.20 1 -2 14 24.40 1.90 -1 -2 -14 20.60 1.90 1 -2 14 22.70 1.80 -1 2 -14 20.70 1.90 1 2 14 21.10 1.90 1 2 14 21.00 2.30 -2 -2 -14 0.10 1.00 2 -2 14 1.90 0.80 2 -2 14 1.00 0.80 2 2 14 1.70 1.00 2 2 14 3.30 1.30 -2 2 -14 2.30 1.10 -3 -2 -14 76.99 3.60 3 -2 14 72.89 3.20 3 -2 14 77.19 3.30 -3 2 -14 72.49 3.60 3 2 14 79.19 3.30 3 2 14 76.79 3.30 4 -2 14 31.40 2.70 4 -2 14 38.40 2.00 -4 -2 -14 39.10 2.50 4 2 14 41.00 2.00 4 2 14 38.00 2.00 5 -2 14 53.79 2.40 5 2 14 54.69 2.40 5 2 14 54.89 2.60 6 -2 14 3.90 0.80 6 2 14 2.40 0.70 8 3 -14 197.38 6.80 8 3 -14 192.18 6.70 7 3 -14 131.49 4.70 7 3 -14 131.59 4.80 6 -3 -14 143.19 5.70 -6 -3 14 142.49 5.30 6 3 -14 146.19 5.30 6 3 -14 146.79 5.40 -5 -3 14 307.17 10.80 5 -3 -14 313.47 11.10 5 3 -14 309.67 10.80 5 3 -14 309.57 10.70 -4 -3 14 115.09 4.50 4 -3 -14 112.29 4.70 -4 3 14 115.39 4.50 4 3 -14 115.49 4.50 4 3 -14 113.19 4.40 3 -3 -14 396.86 14.40 -3 -3 14 414.76 14.40 -3 3 14 406.46 14.10 3 3 -14 412.96 14.10 -2 -3 14 5.50 1.20 2 -3 -14 4.80 1.30 2 3 -14 6.90 1.10 -1 -3 14 40.30 2.20 1 -3 -14 40.30 2.40 -1 3 14 40.20 2.50 1 3 -14 42.70 2.20 0 -3 -14 52.39 2.80 0 -3 14 54.19 2.60 0 3 -14 56.09 2.60 0 3 14 53.59 2.70 -1 -3 -14 34.20 2.20 1 -3 14 33.50 2.00 1 -3 14 33.20 2.10 -1 3 -14 35.30 2.00 1 3 14 32.50 2.00 2 -3 14 134.69 5.20 2 -3 14 138.99 5.20 -2 -3 -14 138.39 5.60 2 3 14 139.59 5.30 -2 3 -14 140.89 5.20 2 3 14 135.79 5.30 -3 -3 -14 254.87 9.10 3 -3 14 250.07 8.70 -3 3 -14 233.58 8.90 3 3 14 253.97 8.80 3 3 14 240.68 8.90 4 -3 14 72.19 3.20 4 3 14 73.29 3.10 4 3 14 77.39 3.10 -4 3 -14 77.99 3.10 5 -3 14 24.00 1.30 5 3 14 25.90 1.50 6 4 -14 5.20 1.00 6 4 -14 3.10 0.80 -5 -4 14 -0.20 0.70 5 4 -14 -1.10 0.70 5 4 -14 0.70 0.50 -4 -4 14 1.50 0.60 4 -4 -14 1.90 0.90 4 4 -14 2.40 0.80 4 4 -14 2.20 0.80 -4 4 14 1.40 1.00 -3 -4 14 1.60 0.60 3 -4 -14 4.00 1.30 3 4 -14 1.50 0.50 -3 4 14 2.10 1.00 2 -4 -14 9.80 1.40 -2 4 14 8.40 1.20 2 4 -14 7.30 1.00 1 -4 -14 13.30 1.50 -1 -4 14 9.50 1.20 -1 4 14 12.40 1.30 1 4 -14 11.80 1.10 0 -4 -14 -0.60 0.80 0 -4 14 1.40 0.60 0 4 14 0.20 0.80 0 4 -14 0.20 0.50 1 -4 14 85.09 3.70 -1 -4 -14 97.09 4.00 1 -4 14 94.09 3.80 1 4 14 88.79 3.70 -1 4 -14 95.69 3.60 2 -4 14 8.60 1.20 2 -4 14 9.20 1.20 -2 4 -14 7.80 0.90 3 -4 14 10.30 1.10 3 4 14 12.10 1.30 -3 4 -14 11.70 1.10 4 -4 14 14.30 1.10 -1 -5 14 110.19 4.10 1 5 -14 115.49 4.10 -1 5 14 113.89 4.20 0 5 -14 3.30 0.70 -6 0 15 -0.20 1.30 -5 0 15 -0.20 0.80 -4 0 15 -0.10 0.70 -3 0 15 0.30 0.70 -2 0 15 -0.40 0.70 -1 0 15 -1.40 0.70 0 0 15 0.10 0.70 1 0 15 -0.10 0.70 2 0 15 2.20 1.10 2 0 15 0.00 0.70 3 0 15 -0.40 0.90 3 0 15 -0.60 0.70 4 0 15 0.70 0.90 4 0 15 0.30 0.90 5 0 15 0.50 0.60 -6 -1 15 20.00 1.90 -5 -1 15 17.00 1.60 5 -1 -15 20.10 2.50 -5 1 15 19.80 1.70 4 -1 -15 72.09 3.80 -4 -1 15 80.89 3.40 -4 1 15 81.19 3.40 -3 -1 15 180.58 6.70 3 -1 -15 175.48 7.00 -3 1 15 186.08 6.80 -2 -1 15 1.50 0.70 2 -1 -15 2.30 1.40 -2 1 15 2.60 0.80 -1 -1 15 124.09 4.90 1 -1 -15 120.19 5.30 -1 1 15 128.99 6.20 0 -1 15 310.07 11.20 0 1 15 324.77 12.00 1 -1 15 48.30 2.40 1 1 15 45.00 2.50 2 -1 15 17.60 1.60 2 -1 15 18.70 1.50 2 1 15 18.00 1.50 3 -1 15 73.59 3.10 3 -1 15 70.89 3.10 3 1 15 73.99 3.60 3 1 15 78.29 3.20 4 -1 15 1.50 1.00 4 -1 15 3.60 1.00 4 1 15 3.70 0.80 4 1 15 1.10 0.80 5 -1 15 1.30 0.60 5 1 15 3.10 1.00 6 2 -15 4.80 1.30 5 -2 -15 61.09 3.00 -5 -2 15 60.49 2.70 -5 2 15 59.79 2.80 5 2 -15 59.09 2.70 4 -2 -15 160.68 6.10 -4 -2 15 152.08 5.70 -4 2 15 158.58 5.80 4 2 -15 148.49 5.70 -3 -2 15 11.20 1.30 3 -2 -15 9.00 1.60 3 2 -15 8.20 1.80 -3 2 15 10.60 1.40 2 -2 -15 26.30 2.10 -2 -2 15 28.00 2.00 -2 2 15 24.00 1.70 2 2 -15 21.90 2.10 1 -2 -15 63.09 3.10 -1 -2 15 63.39 3.20 -1 2 15 61.19 2.90 1 2 -15 53.49 4.10 0 -2 -15 3.60 1.30 0 2 15 0.90 0.80 1 -2 15 -0.20 0.60 -1 -2 -15 1.50 1.30 1 2 15 0.60 0.70 2 -2 15 69.09 3.00 2 -2 15 67.59 3.00 2 2 15 77.49 4.00 3 -2 15 -0.10 0.80 3 -2 15 1.00 0.80 3 2 15 0.40 1.00 3 2 15 -0.30 0.70 4 -2 15 5.40 1.00 4 2 15 6.60 1.20 4 2 15 7.90 1.40 5 -2 15 2.70 0.70 6 3 -15 5.10 1.00 -5 -3 15 8.10 1.20 5 3 -15 8.80 1.10 4 3 -15 11.30 1.10 -4 3 15 10.30 1.60 3 -3 -15 101.29 4.40 -3 -3 15 105.79 4.10 3 3 -15 106.39 4.00 -2 -3 15 16.30 1.40 2 -3 -15 14.80 1.70 2 3 -15 16.10 1.30 -2 3 15 15.50 1.30 -1 -3 15 0.50 0.60 1 -3 -15 -1.40 1.10 1 3 -15 0.40 0.70 -1 3 15 0.60 0.60 0 -3 -15 20.00 1.90 0 -3 15 21.20 1.40 0 3 15 23.70 2.00 0 3 -15 20.90 1.50 -1 3 -15 1.80 0.80 1 3 15 1.70 0.60 2 -3 15 35.40 1.80 2 3 15 34.40 1.80 3 3 15 -0.60 0.70 -3 -4 15 7.40 1.00 3 4 -15 8.90 1.00 -2 -4 15 89.59 3.40 2 4 -15 87.29 3.30 -2 4 15 87.29 3.40 -1 -4 15 11.20 1.00 -1 4 15 9.50 1.10 1 4 -15 10.70 1.10 0 -4 15 22.90 1.30 0 4 15 24.40 1.40 0 4 -15 22.30 1.50 -5 0 16 112.69 4.30 -4 0 16 33.40 2.00 -3 0 16 54.49 2.50 -2 0 16 55.29 2.90 -1 0 16 639.04 21.60 0 0 16 1313.57 44.20 1 0 16 54.99 2.50 2 0 16 67.89 2.80 3 0 16 28.50 1.70 -5 -1 16 0.40 0.90 -4 -1 16 8.50 1.20 -4 1 16 9.80 1.40 -3 -1 16 1.80 0.60 -3 1 16 1.20 0.70 -2 -1 16 27.40 1.70 -2 1 16 26.00 2.40 -1 1 16 4.80 1.10 0 -1 16 5.90 1.40 0 1 16 4.20 1.00 1 1 16 111.09 4.50 2 -1 16 10.90 1.30 2 1 16 8.90 1.10 3 1 16 11.00 2.00 -4 -2 16 2.50 0.70 -4 2 16 6.50 1.50 -3 -2 16 1.10 0.60 -3 2 16 0.40 0.70 -2 2 16 4.80 1.00 -1 2 16 40.40 2.40 0 -2 16 16.30 1.30 0 2 16 16.70 1.20 1 -2 16 10.30 1.10 1 2 16 8.90 1.10 2 -2 16 36.00 2.40 2 2 16 28.60 1.60 -2 -3 16 17.60 1.20 -2 3 16 18.00 1.30 -1 -3 16 11.00 1.00 -1 3 16 7.30 1.10 -2 0 17 -0.30 0.60 -1 0 17 0.70 0.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 11462 _shelx_res_file ; TITL jtm1198_0m_a.res in P2(1)/c jtm1198_0m_a.res created by SHELXL-2018/3 at 15:50:21 on 31-Dec-2019 REM Old TITL jtm1198_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.103, Rweak 0.003, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C14 N3 S CELL 1.54178 12.4617 7.0766 13.6500 90.000 96.085 90.000 ZERR 4.000 0.0005 0.0003 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N S UNIT 52 48 16 4 TEMP -123 SIZE 0.156 0.218 0.257 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 MPLA N1 > C5 MPLA C7 > C12 CONF EQIV $1 x, y-1, z HTAB C2 S1_$1 ACTA 136 WGHT 0.079200 0.912600 EXTI 0.017523 FVAR 0.84588 S1 4 0.651899 0.561758 0.632805 11.00000 0.02359 0.02297 = 0.03413 -0.00033 0.00211 0.00000 N1 3 0.602371 0.196645 0.624618 11.00000 0.02252 0.02112 = 0.03267 0.00088 0.00388 0.00114 N2 3 0.425034 0.058013 0.619204 11.00000 0.02587 0.01983 = 0.02955 -0.00025 0.00422 -0.00093 N3 3 0.284644 0.292082 0.620892 11.00000 0.01941 0.02515 = 0.02603 -0.00131 0.00209 -0.00167 N4 3 0.277152 0.485131 0.624267 11.00000 0.02416 0.02509 = 0.02931 -0.00336 0.00243 0.00219 C1 1 0.562833 0.371829 0.628218 11.00000 0.02110 0.02139 = 0.01785 0.00098 0.00060 -0.00224 C2 1 0.530489 0.051913 0.620473 11.00000 0.02813 0.01909 = 0.03873 -0.00115 0.00395 0.00236 H2 2 0.561282 -0.074017 0.617859 11.00000 0.04034 C3 1 0.388196 0.237101 0.622097 11.00000 0.02136 0.02425 = 0.01945 -0.00056 0.00184 -0.00338 C4 1 0.376309 0.552438 0.628050 11.00000 0.02266 0.02422 = 0.02807 -0.00309 0.00227 0.00376 H4 2 0.387187 0.676157 0.632570 11.00000 0.01597 C5 1 0.451911 0.401433 0.626844 11.00000 0.02245 0.01969 = 0.02156 -0.00157 0.00117 -0.00031 C6 1 0.188602 0.171090 0.614040 11.00000 0.02009 0.03198 = 0.02462 0.00020 0.00454 -0.00668 H6A 2 0.213160 0.050482 0.636932 11.00000 0.02411 H6B 2 0.143881 0.215046 0.659384 11.00000 0.02429 C7 1 0.131009 0.162652 0.511104 11.00000 0.01611 0.02001 = 0.02549 0.00097 0.00363 -0.00289 C8 1 0.177187 0.066050 0.437087 11.00000 0.01904 0.02162 = 0.02942 0.00024 0.00473 0.00044 H8 2 0.241524 0.004411 0.450707 11.00000 0.02051 C9 1 0.124223 0.057493 0.342451 11.00000 0.03017 0.02499 = 0.02724 -0.00374 0.00765 -0.00504 H9 2 0.156336 -0.002554 0.295107 11.00000 0.03837 C10 1 0.024995 0.145632 0.321151 11.00000 0.02647 0.03292 = 0.02728 0.00479 -0.00358 -0.00992 H10 2 -0.003928 0.137278 0.263663 11.00000 0.04134 C11 1 -0.021574 0.242330 0.394110 11.00000 0.01635 0.02992 = 0.04002 0.00815 -0.00078 -0.00134 H11 2 -0.082479 0.299439 0.380085 11.00000 0.03265 C12 1 0.031666 0.250639 0.488944 11.00000 0.01871 0.02192 = 0.03367 0.00017 0.00659 -0.00117 H12 2 -0.002536 0.320544 0.538318 11.00000 0.04111 C13 1 0.778785 0.443998 0.631622 11.00000 0.02559 0.02960 = 0.04413 0.00388 -0.00026 -0.00200 H13A 2 0.780893 0.380843 0.570017 11.00000 0.04010 H13B 2 0.786722 0.361071 0.686214 11.00000 0.03578 H13C 2 0.836037 0.547433 0.632827 11.00000 0.06757 HKLF 4 REM jtm1198_0m_a.res in P2(1)/c REM wR2 = 0.134862, GooF = S = 1.09953, Restrained GooF = 1.09953 for all data REM R1 = 0.048725 for 2292 Fo > 4sig(Fo) and 0.049755 for all 2388 data REM 212 parameters refined using 0 restraints END WGHT 0.0792 0.9126 REM Highest difference peak 0.684, deepest hole -0.419, 1-sigma level 0.083 Q1 1 0.6659 0.3466 0.6422 11.00000 0.05 0.68 Q2 1 0.7355 0.5253 0.6368 11.00000 0.05 0.42 Q3 1 0.3637 -0.0080 0.6219 11.00000 0.05 0.35 Q4 1 0.0046 0.1901 0.3634 11.00000 0.05 0.34 Q5 1 0.0793 0.0982 0.3408 11.00000 0.05 0.32 ; _shelx_res_checksum 58812 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 0.65190(4) 0.56176(7) 0.63280(4) 0.0270(2) Uani d 1 . . N N1 0.60237(13) 0.1966(2) 0.62462(13) 0.0254(4) Uani d 1 . . N N2 0.42503(15) 0.0580(2) 0.61920(13) 0.0250(4) Uani d 1 . . N N3 0.28464(13) 0.2921(2) 0.62089(12) 0.0236(4) Uani d 1 . . N N4 0.27715(14) 0.4851(3) 0.62427(13) 0.0262(4) Uani d 1 . . C C1 0.56283(15) 0.3718(3) 0.62822(13) 0.0202(4) Uani d 1 . . C C2 0.53049(18) 0.0519(3) 0.62047(17) 0.0286(5) Uani d 1 . . H H2 0.561(2) -0.074(4) 0.618(2) 0.040(8) Uiso d 1 . . C C3 0.38820(15) 0.2371(3) 0.62210(13) 0.0217(4) Uani d 1 . . C C4 0.37631(17) 0.5524(3) 0.62805(15) 0.0250(4) Uani d 1 . . H H4 0.3872(18) 0.676(4) 0.6326(16) 0.016(5) Uiso d 1 . . C C5 0.45191(16) 0.4014(3) 0.62684(14) 0.0213(4) Uani d 1 . . C C6 0.18860(16) 0.1711(3) 0.61404(14) 0.0254(4) Uani d 1 . . H H6A 0.213(2) 0.050(4) 0.6369(18) 0.024(6) Uiso d 1 . . H H6B 0.144(2) 0.215(4) 0.6594(18) 0.024(6) Uiso d 1 . . C C7 0.13101(14) 0.1627(3) 0.51110(13) 0.0204(4) Uani d 1 . . C C8 0.17719(16) 0.0661(3) 0.43709(15) 0.0232(4) Uani d 1 . . H H8 0.242(2) 0.004(4) 0.4507(16) 0.021(5) Uiso d 1 . . C C9 0.12422(18) 0.0575(3) 0.34245(16) 0.0271(5) Uani d 1 . . H H9 0.156(2) -0.003(4) 0.295(2) 0.038(7) Uiso d 1 . . C C10 0.02500(17) 0.1456(3) 0.32115(16) 0.0293(5) Uani d 1 . . H H10 -0.004(2) 0.137(4) 0.264(2) 0.041(8) Uiso d 1 . . C C11 -0.02157(16) 0.2423(3) 0.39411(16) 0.0290(5) Uani d 1 . . H H11 -0.082(2) 0.299(4) 0.3801(19) 0.033(7) Uiso d 1 . . C C12 0.03167(15) 0.2506(3) 0.48894(15) 0.0245(4) Uani d 1 . . H H12 -0.003(2) 0.321(4) 0.538(2) 0.041(7) Uiso d 1 . . C C13 0.77879(19) 0.4440(3) 0.6316(2) 0.0334(5) Uani d 1 . . H H13A 0.781(2) 0.381(4) 0.570(2) 0.040(7) Uiso d 1 . . H H13B 0.787(2) 0.361(4) 0.686(2) 0.036(7) Uiso d 1 . . H H13C 0.836(3) 0.547(5) 0.633(3) 0.068(11) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0236(3) 0.0230(3) 0.0341(3) 0.00000(17) 0.0021(2) -0.00033(17) N1 0.0225(8) 0.0211(8) 0.0327(9) 0.0011(6) 0.0039(7) 0.0009(6) N2 0.0259(9) 0.0198(8) 0.0295(9) -0.0009(6) 0.0042(7) -0.0002(6) N3 0.0194(8) 0.0252(9) 0.0260(8) -0.0017(6) 0.0021(6) -0.0013(6) N4 0.0242(9) 0.0251(9) 0.0293(8) 0.0022(7) 0.0024(6) -0.0034(7) C1 0.0211(9) 0.0214(9) 0.0178(8) -0.0022(7) 0.0006(6) 0.0010(7) C2 0.0281(11) 0.0191(10) 0.0387(12) 0.0024(8) 0.0039(9) -0.0011(8) C3 0.0214(9) 0.0242(10) 0.0194(8) -0.0034(7) 0.0018(7) -0.0006(7) C4 0.0227(10) 0.0242(11) 0.0281(10) 0.0038(7) 0.0023(8) -0.0031(7) C5 0.0224(10) 0.0197(9) 0.0216(9) -0.0003(7) 0.0012(7) -0.0016(7) C6 0.0201(9) 0.0320(11) 0.0246(9) -0.0067(8) 0.0045(8) 0.0002(8) C7 0.0161(8) 0.0200(8) 0.0255(9) -0.0029(7) 0.0036(7) 0.0010(7) C8 0.0190(10) 0.0216(9) 0.0294(10) 0.0004(7) 0.0047(8) 0.0002(7) C9 0.0302(11) 0.0250(10) 0.0272(10) -0.0050(8) 0.0076(8) -0.0037(7) C10 0.0265(10) 0.0329(11) 0.0273(10) -0.0099(8) -0.0036(8) 0.0048(8) C11 0.0164(9) 0.0299(11) 0.0400(11) -0.0013(8) -0.0008(8) 0.0082(9) C12 0.0187(9) 0.0219(9) 0.0337(10) -0.0012(7) 0.0066(7) 0.0002(7) C13 0.0256(11) 0.0296(12) 0.0441(13) -0.0020(8) -0.0003(9) 0.0039(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 S1 C13 . . 101.59(10) ? C1 N1 C2 . . 117.19(17) ? C2 N2 C3 . . 111.93(17) ? C3 N3 N4 . . 110.87(16) ? C3 N3 C6 . . 127.36(18) ? N4 N3 C6 . . 121.74(16) ? C4 N4 N3 . . 107.11(16) ? N1 C1 C5 . . 120.45(17) ? N1 C1 S1 . . 118.78(15) ? C5 C1 S1 . . 120.76(15) ? N2 C2 N1 . . 129.09(19) ? N2 C2 H2 . . 115.3(18) ? N1 C2 H2 . . 115.6(18) ? N3 C3 N2 . . 126.83(18) ? N3 C3 C5 . . 107.31(18) ? N2 C3 C5 . . 125.86(18) ? N4 C4 C5 . . 110.24(18) ? N4 C4 H4 . . 119.6(15) ? C5 C4 H4 . . 130.1(15) ? C1 C5 C3 . . 115.47(18) ? C1 C5 C4 . . 140.06(19) ? C3 C5 C4 . . 104.47(17) ? N3 C6 C7 . . 112.75(15) ? N3 C6 H6A . . 105.8(16) ? C7 C6 H6A . . 112.1(15) ? N3 C6 H6B . . 107.8(15) ? C7 C6 H6B . . 111.9(15) ? H6A C6 H6B . . 106(2) ? C12 C7 C8 . . 119.25(18) ? C12 C7 C6 . . 120.62(17) ? C8 C7 C6 . . 120.13(17) ? C9 C8 C7 . . 120.25(19) ? C9 C8 H8 . . 119.2(14) ? C7 C8 H8 . . 120.5(14) ? C10 C9 C8 . . 120.03(19) ? C10 C9 H9 . . 121.0(18) ? C8 C9 H9 . . 119.0(18) ? C11 C10 C9 . . 120.2(2) ? C11 C10 H10 . . 123(2) ? C9 C10 H10 . . 117(2) ? C10 C11 C12 . . 119.65(19) ? C10 C11 H11 . . 119.8(18) ? C12 C11 H11 . . 120.5(18) ? C7 C12 C11 . . 120.61(19) ? C7 C12 H12 . . 121.6(17) ? C11 C12 H12 . . 117.8(17) ? S1 C13 H13A . . 109.4(17) ? S1 C13 H13B . . 107.5(17) ? H13A C13 H13B . . 113(3) ? S1 C13 H13C . . 106(2) ? H13A C13 H13C . . 105(3) ? H13B C13 H13C . . 115(3) ? 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 C1 . 1.7400(19) ? S1 C13 . 1.789(2) ? N1 C1 . 1.337(3) ? N1 C2 . 1.358(3) ? N2 C2 . 1.313(3) ? N2 C3 . 1.350(3) ? N3 C3 . 1.346(3) ? N3 N4 . 1.370(2) ? N3 C6 . 1.466(2) ? N4 C4 . 1.320(3) ? C1 C5 . 1.396(3) ? C2 H2 . 0.97(3) ? C3 C5 . 1.406(3) ? C4 C5 . 1.426(3) ? C4 H4 . 0.89(2) ? C6 C7 . 1.510(3) ? C6 H6A . 0.95(3) ? C6 H6B . 0.93(3) ? C7 C12 . 1.390(3) ? C7 C8 . 1.394(3) ? C8 C9 . 1.388(3) ? C8 H8 . 0.91(2) ? C9 C10 . 1.388(3) ? C9 H9 . 0.90(3) ? C10 C11 . 1.385(3) ? C10 H10 . 0.83(3) ? C11 C12 . 1.392(3) ? C11 H11 . 0.86(3) ? C12 H12 . 0.97(3) ? C13 H13A . 0.96(3) ? C13 H13B . 0.95(3) ? C13 H13C . 1.02(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C2 H2 S1 1_545 0.97(3) 2.81(3) 3.781(2) 174(2) yes C13 H13C Cg3 3_666 1.02(4) 2.49(4) 3.455(2) 157(3) y 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 C3 N3 N4 C4 . . . . -0.3(2) ? C6 N3 N4 C4 . . . . -178.65(17) ? C2 N1 C1 C5 . . . . -0.5(3) ? C2 N1 C1 S1 . . . . -179.60(15) ? C13 S1 C1 N1 . . . . -0.32(18) ? C13 S1 C1 C5 . . . . -179.38(17) ? C3 N2 C2 N1 . . . . 0.3(3) ? C1 N1 C2 N2 . . . . 0.2(3) ? N4 N3 C3 N2 . . . . -179.71(18) ? C6 N3 C3 N2 . . . . -1.4(3) ? N4 N3 C3 C5 . . . . 0.2(2) ? C6 N3 C3 C5 . . . . 178.49(16) ? C2 N2 C3 N3 . . . . 179.36(19) ? C2 N2 C3 C5 . . . . -0.6(3) ? N3 N4 C4 C5 . . . . 0.2(2) ? N1 C1 C5 C3 . . . . 0.3(3) ? S1 C1 C5 C3 . . . . 179.39(13) ? N1 C1 C5 C4 . . . . -179.1(2) ? S1 C1 C5 C4 . . . . 0.0(3) ? N3 C3 C5 C1 . . . . -179.69(16) ? N2 C3 C5 C1 . . . . 0.2(3) ? N3 C3 C5 C4 . . . . -0.1(2) ? N2 C3 C5 C4 . . . . 179.84(18) ? N4 C4 C5 C1 . . . . 179.4(2) ? N4 C4 C5 C3 . . . . -0.1(2) ? C3 N3 C6 C7 . . . . -99.9(2) ? N4 N3 C6 C7 . . . . 78.2(2) ? N3 C6 C7 C12 . . . . -108.9(2) ? N3 C6 C7 C8 . . . . 71.1(2) ? C12 C7 C8 C9 . . . . -0.2(3) ? C6 C7 C8 C9 . . . . 179.77(18) ? C7 C8 C9 C10 . . . . 0.1(3) ? C8 C9 C10 C11 . . . . 0.0(3) ? C9 C10 C11 C12 . . . . 0.0(3) ? C8 C7 C12 C11 . . . . 0.2(3) ? C6 C7 C12 C11 . . . . -179.80(18) ? C10 C11 C12 C7 . . . . -0.1(3) ?