#------------------------------------------------------------------------------ #$Date: 2024-06-01 05:25:57 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292165 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571767.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_1571767 loop_ _publ_author_name 'Waters, James K.' 'Kelley, Steven P.' 'Mossine, Valeri V.' 'Mawhinney, Thomas P.' _publ_section_title ; (S)-2-Carboxyethyl L-cysteinyl sulfone ; _journal_coeditor_code PK4044 _journal_issue 5 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624004802 _journal_volume 9 _journal_year 2024 _chemical_absolute_configuration rmad _chemical_formula_iupac 'C6 H11 N O6 S' _chemical_formula_moiety 'C6 H11 N O6 S' _chemical_formula_sum 'C6 H11 N O6 S' _chemical_formula_weight 225.22 _chemical_name_common ; (S)-2-Carboxyethyl L-cysteinyl sulfone ; _chemical_name_systematic ; (2S)-2-Azaniumyl-3-[(2-carboxyethane)sulfonyl]propanoate ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 110.3246(16) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.8838(2) _cell_length_b 18.3867(7) _cell_length_c 5.1522(2) _cell_measurement_reflns_used 9939 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 30.56 _cell_measurement_theta_min 3.32 _cell_volume 433.85(3) _computing_cell_refinement ; APEX3 V.2018.1-0 and SAINT V8.38A (Bruker, 2014) ; _computing_data_collection ; APEX3 V.2018.1-0 (Bruker, 2014) ; _computing_data_reduction ; APEX3 V.2018.1-0 and SAINT V8.38A (Bruker, 2014) ; _computing_molecular_graphics ; CrystalExplorer 17.5 (Mackenzie et al., 2017), Mercury (Macrae et al., 2020) ; _computing_publication_material ; Olex2 (Dolomanov et al., 2009), and publCIF (Westrip, 2010) ; _computing_structure_refinement ; ShelXL (Sheldrick, 2015) ; _computing_structure_solution ; ShelXS (Sheldrick, 2008) ; _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEXII area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_unetI/netI 0.0108 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 15133 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.571 _diffrn_reflns_theta_min 2.215 _diffrn_source 'Sealed Source Mo with TRIUMPH optics' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.7047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (AXScale; Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.724 _exptl_crystal_description plate _exptl_crystal_F_000 236 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.314 _refine_diff_density_min -0.179 _refine_ls_abs_structure_details ; Flack x determined using 1277 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.001(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 2656 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.102 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0189 _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^)+(0.0333P)^2^+0.0609P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0508 _reflns_number_gt 2644 _reflns_number_total 2656 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file pk4044.cif _cod_data_source_block I _cod_database_code 1571767 _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 0.848 _shelx_estimated_absorpt_t_max 0.992 _shelx_hkl_file ; 1 0 0 4.68 0.11 -1 0 0 4.56 0.11 2 0 0 4.40 0.14 -2 0 0 4.80 0.17 -2 0 0 4.25 0.14 -2 0 0 4.58 0.13 2 0 0 4.43 0.15 2 0 0 4.44 0.14 3 0 0 15.21 0.27 3 0 0 14.64 0.34 3 0 0 14.81 0.35 -3 0 0 15.36 0.31 3 0 0 14.81 0.33 3 0 0 14.79 0.33 -3 0 0 14.99 0.34 -3 0 0 14.76 0.36 4 0 0 0.17 0.08 4 0 0 0.23 0.08 -4 0 0 0.10 0.06 -4 0 0 0.29 0.09 4 0 0 0.09 0.07 -4 0 0 0.22 0.10 -4 0 0 0.17 0.08 -5 0 0 1.52 0.17 -5 0 0 1.79 0.17 5 0 0 1.90 0.17 5 0 0 1.95 0.17 5 0 0 1.32 0.16 -5 0 0 1.45 0.19 -6 0 0 2.10 0.22 6 0 0 2.09 0.23 6 0 0 2.41 0.22 -6 0 0 2.02 0.24 6 0 0 2.13 0.21 -6 0 0 2.33 0.26 0 -1 0 0.42 0.02 0 1 0 0.00 0.00 -1 -1 0 163.06 2.47 1 -1 0 159.35 2.42 -1 1 0 158.98 2.46 -1 1 0 167.81 2.48 1 1 0 164.88 2.45 2 -1 0 128.15 1.98 -2 -1 0 131.80 1.99 2 -1 0 128.34 1.99 -2 -1 0 125.39 2.01 2 -1 0 130.94 1.95 2 -1 0 125.41 1.98 -2 -1 0 132.39 1.98 2 -1 0 129.55 2.00 -2 -1 0 132.20 2.04 2 1 0 130.14 2.06 -2 1 0 133.46 2.07 -2 1 0 135.37 2.08 2 1 0 132.81 2.06 -2 1 0 136.64 2.10 2 1 0 131.03 2.06 2 1 0 134.35 2.08 -2 1 0 140.26 2.06 3 -1 0 24.54 0.47 -3 -1 0 24.57 0.52 3 -1 0 25.04 0.49 3 -1 0 24.42 0.48 3 -1 0 24.97 0.42 -3 -1 0 24.10 0.54 -3 -1 0 24.93 0.49 -3 -1 0 24.92 0.47 3 -1 0 24.89 0.50 -3 1 0 24.57 0.44 3 1 0 23.25 0.49 3 1 0 23.39 0.47 -3 1 0 24.10 0.49 -3 1 0 24.14 0.52 3 1 0 24.08 0.47 3 1 0 24.13 0.48 -3 1 0 24.24 0.49 4 -1 0 9.41 0.30 -4 -1 0 9.57 0.32 4 -1 0 9.21 0.29 -4 -1 0 9.56 0.26 4 -1 0 9.28 0.28 -4 -1 0 9.57 0.29 -4 -1 0 8.93 0.33 -4 1 0 9.27 0.30 4 1 0 9.00 0.28 4 1 0 8.89 0.28 -4 1 0 8.95 0.29 -4 1 0 9.02 0.33 5 -1 0 59.17 1.11 -5 -1 0 60.94 1.12 -5 -1 0 58.04 1.20 5 -1 0 58.71 1.10 -5 -1 0 59.10 1.16 5 -1 0 59.52 1.14 -5 1 0 60.49 1.13 -5 1 0 59.75 1.14 5 1 0 59.47 1.11 5 1 0 58.39 1.14 5 1 0 59.71 1.11 -5 1 0 59.09 1.17 -5 1 0 60.00 1.21 6 -1 0 6.62 0.31 -6 -1 0 6.69 0.36 -6 -1 0 6.10 0.33 6 -1 0 6.12 0.32 -6 -1 0 6.56 0.38 6 -1 0 6.76 0.30 -6 1 0 6.42 0.37 -6 1 0 7.18 0.34 -6 1 0 6.63 0.36 6 1 0 5.99 0.31 6 1 0 6.63 0.30 6 1 0 6.67 0.34 0 -2 0 44.79 0.69 0 2 0 46.52 0.71 1 -2 0 169.30 2.61 -1 -2 0 177.37 2.63 1 -2 0 175.33 2.64 1 2 0 168.49 2.57 -1 2 0 174.36 2.60 -1 2 0 170.90 2.60 -2 -2 0 162.55 2.55 -2 -2 0 169.08 2.51 2 -2 0 165.20 2.52 2 -2 0 163.34 2.52 2 -2 0 167.09 2.48 2 -2 0 164.82 2.51 2 -2 0 164.23 2.50 -2 -2 0 163.93 2.51 2 2 0 161.03 2.50 2 2 0 159.38 2.49 2 2 0 162.19 2.51 -2 2 0 161.22 2.51 -2 2 0 170.72 2.53 2 2 0 166.13 2.50 -2 2 0 165.41 2.50 3 -2 0 0.27 0.04 -3 -2 0 0.18 0.06 -3 -2 0 0.33 0.08 3 -2 0 0.45 0.06 -3 -2 0 0.39 0.06 3 -2 0 0.33 0.05 3 -2 0 0.20 0.06 3 -2 0 0.15 0.06 3 -2 0 0.18 0.06 -3 -2 0 0.13 0.07 -3 -2 0 0.20 0.06 3 2 0 0.38 0.07 -3 2 0 0.49 0.06 3 2 0 0.33 0.07 3 2 0 0.37 0.07 -3 2 0 0.36 0.07 -3 2 0 0.34 0.08 3 2 0 0.35 0.06 -4 -2 0 21.15 0.55 4 -2 0 21.19 0.49 -4 -2 0 21.05 0.52 4 -2 0 20.72 0.47 -4 -2 0 20.79 0.45 -4 -2 0 21.24 0.48 4 -2 0 21.64 0.48 -4 2 0 21.13 0.52 -4 2 0 21.46 0.49 4 2 0 20.41 0.47 -4 2 0 21.87 0.54 4 2 0 21.63 0.48 4 2 0 21.20 0.50 -4 2 0 21.45 0.50 -5 -2 0 15.92 0.52 -5 -2 0 15.38 0.47 5 -2 0 16.34 0.44 5 -2 0 15.73 0.46 5 -2 0 15.65 0.43 -5 -2 0 16.33 0.44 5 2 0 15.59 0.43 5 2 0 15.39 0.46 -5 2 0 16.19 0.50 -5 2 0 15.86 0.45 -5 2 0 15.60 0.48 5 2 0 15.52 0.43 -5 2 0 15.80 0.45 -6 -2 0 29.26 0.75 -6 -2 0 28.86 0.80 6 -2 0 28.83 0.70 6 -2 0 28.40 0.69 -6 2 0 27.28 0.77 -6 2 0 28.93 0.75 6 2 0 28.38 0.73 6 2 0 28.41 0.68 6 2 0 28.55 0.69 0 -3 0 1.16 0.06 1 -3 0 449.91 6.93 -1 -3 0 460.61 6.95 -1 -3 0 472.56 6.90 1 -3 0 437.47 6.83 1 -3 0 452.74 7.11 -1 -3 0 450.49 6.88 1 3 0 437.32 6.85 1 3 0 450.18 6.90 -1 3 0 476.99 6.92 1 3 0 445.77 6.83 -1 3 0 450.18 6.88 -2 -3 0 47.77 0.78 2 -3 0 45.83 0.78 2 -3 0 47.03 0.78 2 -3 0 47.41 0.75 2 -3 0 47.24 0.75 -2 -3 0 47.14 0.77 2 -3 0 46.84 0.78 2 3 0 44.75 0.74 -2 3 0 44.85 0.76 2 3 0 43.86 0.74 -2 3 0 43.48 0.76 -2 3 0 45.62 0.73 2 3 0 43.72 0.75 2 3 0 42.91 0.74 -3 -3 0 20.02 0.42 3 -3 0 19.70 0.43 3 -3 0 20.94 0.36 3 -3 0 20.83 0.42 -3 -3 0 20.61 0.36 3 -3 0 20.40 0.38 3 -3 0 20.80 0.36 3 -3 0 20.96 0.43 -3 -3 0 20.09 0.46 -3 -3 0 20.29 0.41 -3 -3 0 20.01 0.48 -3 3 0 19.47 0.44 3 3 0 20.01 0.42 3 3 0 19.95 0.42 -3 3 0 20.41 0.37 3 3 0 20.29 0.44 -3 3 0 20.90 0.42 -3 3 0 20.23 0.44 3 3 0 19.37 0.41 -3 3 0 20.16 0.46 4 -3 0 23.45 0.44 -4 -3 0 22.97 0.48 -4 -3 0 22.56 0.57 4 -3 0 21.83 0.50 -4 -3 0 23.38 0.56 4 -3 0 22.77 0.50 4 -3 0 22.90 0.52 -4 -3 0 22.13 0.49 4 3 0 23.10 0.54 -4 3 0 23.52 0.57 -4 3 0 22.27 0.54 4 3 0 23.72 0.51 -4 3 0 23.18 0.51 4 3 0 23.01 0.51 -4 3 0 23.89 0.53 5 -3 0 3.84 0.22 5 -3 0 3.95 0.22 -5 -3 0 4.06 0.27 -5 -3 0 4.27 0.26 5 -3 0 3.93 0.24 -5 3 0 3.86 0.26 -5 3 0 3.39 0.21 5 3 0 3.45 0.21 -5 3 0 3.76 0.26 -5 3 0 3.60 0.22 5 3 0 3.68 0.23 5 3 0 3.63 0.21 -6 -3 0 34.21 0.90 6 -3 0 35.41 0.79 -6 -3 0 34.46 0.85 6 -3 0 34.61 0.79 6 3 0 33.96 0.77 -6 3 0 33.23 0.84 6 3 0 35.03 0.78 6 3 0 34.90 0.83 -6 3 0 33.96 0.87 0 -4 0 75.93 1.18 0 4 0 70.02 1.09 -1 -4 0 637.17 9.76 1 -4 0 634.34 9.94 -1 -4 0 645.48 9.68 -1 -4 0 649.55 9.64 1 -4 0 662.52 9.65 1 -4 0 628.23 9.76 1 -4 0 624.11 9.69 1 4 0 626.88 9.77 1 4 0 662.79 9.77 1 4 0 628.40 9.68 1 4 0 652.82 9.84 -1 4 0 654.98 9.73 1 4 0 624.73 9.70 -1 4 0 645.75 9.88 2 -4 0 8.85 0.18 2 -4 0 8.98 0.21 -2 -4 0 9.11 0.19 -2 -4 0 8.76 0.21 2 -4 0 9.16 0.20 -2 -4 0 9.04 0.24 2 -4 0 8.95 0.21 -2 -4 0 8.69 0.22 2 -4 0 8.95 0.22 2 -4 0 8.83 0.19 -2 4 0 8.81 0.23 2 4 0 8.73 0.21 -2 4 0 9.08 0.20 2 4 0 8.77 0.21 -2 4 0 8.99 0.23 2 4 0 8.70 0.22 3 -4 0 13.04 0.28 3 -4 0 12.65 0.32 3 -4 0 13.70 0.26 -3 -4 0 12.71 0.37 -3 -4 0 13.45 0.27 -3 -4 0 13.80 0.32 3 -4 0 13.60 0.31 -3 -4 0 13.48 0.31 -3 -4 0 13.38 0.36 3 -4 0 13.32 0.25 3 -4 0 13.22 0.32 -3 4 0 13.64 0.35 3 4 0 13.84 0.32 3 4 0 13.10 0.34 3 4 0 13.42 0.32 -3 4 0 14.32 0.32 -3 4 0 13.24 0.34 -3 4 0 14.02 0.36 -3 4 0 13.66 0.27 -4 -4 0 26.31 0.55 -4 -4 0 25.83 0.61 -4 -4 0 25.42 0.64 4 -4 0 27.07 0.56 4 -4 0 26.57 0.57 4 -4 0 27.06 0.58 -4 -4 0 26.99 0.55 4 -4 0 26.27 0.49 -4 4 0 26.28 0.61 -4 4 0 26.69 0.59 4 4 0 27.21 0.57 4 4 0 26.76 0.56 4 4 0 26.49 0.59 -4 4 0 25.40 0.60 -4 4 0 26.83 0.56 5 -4 0 7.20 0.29 5 -4 0 7.85 0.30 -5 -4 0 7.80 0.34 -5 4 0 7.64 0.34 -5 4 0 7.93 0.31 5 4 0 7.17 0.29 5 4 0 7.39 0.29 5 4 0 7.73 0.32 -5 4 0 7.33 0.33 6 -4 0 9.91 0.38 -6 -4 0 10.20 0.44 -6 -4 0 9.57 0.46 6 -4 0 9.98 0.38 6 4 0 9.41 0.37 -6 4 0 9.38 0.43 -6 4 0 8.73 0.41 6 4 0 9.78 0.36 6 4 0 9.11 0.41 0 -5 0 0.05 0.04 0 -5 0 0.07 0.04 0 5 0 0.09 0.04 -1 -5 0 216.65 3.22 1 -5 0 209.36 3.22 -1 -5 0 215.37 3.29 1 -5 0 217.64 3.22 1 -5 0 215.70 3.23 -1 -5 0 215.80 3.24 -1 -5 0 211.45 3.24 1 5 0 206.51 3.10 -1 5 0 207.61 3.12 1 5 0 204.31 3.10 1 5 0 197.88 3.09 1 5 0 207.86 3.11 1 5 0 208.90 3.10 -1 5 0 212.75 3.11 2 -5 0 153.03 2.35 2 -5 0 149.92 2.34 2 -5 0 154.43 2.31 -2 -5 0 152.04 2.39 2 -5 0 149.70 2.33 -2 -5 0 156.63 2.32 2 -5 0 150.54 2.41 -2 -5 0 152.40 2.33 -2 -5 0 154.19 2.36 -2 5 0 152.97 2.37 2 5 0 150.72 2.35 2 5 0 149.22 2.35 2 5 0 151.55 2.33 -2 5 0 153.80 2.36 2 5 0 151.17 2.34 -2 5 0 155.68 2.35 -2 5 0 151.76 2.34 -3 -5 0 50.97 0.96 3 -5 0 52.47 0.90 -3 -5 0 52.09 0.89 -3 -5 0 53.04 0.98 -3 -5 0 52.69 0.85 3 -5 0 52.13 0.91 3 -5 0 55.18 0.84 3 -5 0 51.58 0.87 3 -5 0 50.55 0.91 -3 -5 0 50.53 0.90 3 -5 0 52.31 0.84 3 5 0 52.08 0.93 -3 5 0 53.31 0.90 -3 5 0 53.06 0.95 3 5 0 51.97 0.91 3 5 0 53.08 0.92 -3 5 0 54.15 0.95 3 5 0 53.90 0.95 -3 5 0 51.99 0.94 -4 -5 0 71.77 1.34 -4 -5 0 74.36 1.27 4 -5 0 73.65 1.29 4 -5 0 74.67 1.28 -4 -5 0 73.37 1.38 4 -5 0 77.05 1.21 -4 -5 0 72.93 1.26 4 -5 0 74.19 1.29 4 5 0 75.77 1.30 -4 5 0 77.26 1.29 4 5 0 74.35 1.30 -4 5 0 75.57 1.36 -4 5 0 73.71 1.34 -4 5 0 76.33 1.34 4 5 0 75.65 1.34 -5 -5 0 50.33 0.96 5 -5 0 50.98 0.98 -5 -5 0 49.68 1.09 -5 -5 0 50.00 1.05 5 -5 0 51.22 0.99 5 5 0 49.68 0.97 -5 5 0 49.32 1.03 -5 5 0 52.05 1.02 5 5 0 51.09 0.98 -5 5 0 51.35 1.06 5 5 0 50.59 1.03 -6 -5 0 0.73 0.18 -6 -5 0 0.88 0.20 6 -5 0 0.98 0.16 6 -5 0 0.77 0.15 6 5 0 1.31 0.17 -6 5 0 1.01 0.19 6 5 0 1.11 0.16 -6 5 0 1.14 0.20 6 5 0 1.28 0.19 0 -6 0 1000.00 14.22 0 -6 0 910.69 14.42 0 -6 0 906.50 14.31 0 -6 0 964.74 14.25 0 6 0 876.36 13.91 0 6 0 954.24 13.81 0 6 0 913.46 13.94 1 -6 0 123.93 1.96 1 -6 0 124.53 2.01 -1 -6 0 129.54 1.95 -1 -6 0 130.66 1.98 -1 -6 0 130.89 1.98 1 -6 0 126.89 1.95 -1 -6 0 129.74 1.96 -1 6 0 127.08 1.93 1 6 0 126.52 1.92 -1 6 0 123.09 1.94 1 6 0 119.67 1.91 1 6 0 125.04 1.92 1 6 0 129.96 1.93 1 6 0 128.48 1.92 2 -6 0 23.88 0.47 2 -6 0 25.48 0.46 2 -6 0 25.41 0.45 -2 -6 0 25.91 0.46 2 -6 0 24.54 0.53 2 -6 0 24.73 0.46 -2 -6 0 25.08 0.45 -2 -6 0 25.52 0.51 -2 -6 0 25.21 0.48 2 6 0 24.72 0.48 2 6 0 24.74 0.47 2 6 0 25.02 0.47 2 6 0 25.80 0.48 -2 6 0 25.79 0.50 -2 6 0 25.17 0.49 -2 6 0 25.87 0.48 -3 -6 0 38.61 0.69 3 -6 0 38.04 0.67 -3 -6 0 38.88 0.78 3 -6 0 37.89 0.65 3 -6 0 37.81 0.69 -3 -6 0 39.07 0.65 -3 -6 0 37.34 0.75 3 -6 0 37.82 0.71 -3 -6 0 37.75 0.71 -3 6 0 39.18 0.68 -3 6 0 38.22 0.74 -3 6 0 39.38 0.74 3 6 0 38.94 0.71 -3 6 0 38.59 0.74 3 6 0 38.60 0.71 3 6 0 38.90 0.74 4 -6 0 12.37 0.35 -4 -6 0 12.64 0.35 4 -6 0 12.09 0.35 -4 -6 0 12.27 0.40 4 -6 0 12.35 0.30 -4 -6 0 12.87 0.42 -4 -6 0 12.78 0.33 4 6 0 12.22 0.34 -4 6 0 12.21 0.38 -4 6 0 11.88 0.36 4 6 0 12.06 0.33 4 6 0 12.42 0.37 -4 6 0 11.98 0.37 -5 -6 0 3.00 0.25 -5 -6 0 2.87 0.25 5 -6 0 3.09 0.21 5 -6 0 2.75 0.20 -5 -6 0 2.77 0.21 5 6 0 2.54 0.18 5 6 0 2.77 0.20 -5 6 0 2.65 0.21 -5 6 0 2.67 0.23 5 6 0 2.76 0.22 -5 6 0 2.93 0.23 -6 -6 0 2.14 0.27 6 -6 0 1.97 0.20 6 -6 0 2.15 0.21 -6 -6 0 2.41 0.26 6 6 0 1.94 0.19 6 6 0 2.05 0.21 -6 6 0 1.79 0.23 -6 6 0 1.74 0.23 6 6 0 2.19 0.23 0 -7 0 0.24 0.05 1 -7 0 92.37 1.44 1 -7 0 89.04 1.45 -1 -7 0 95.20 1.45 -1 -7 0 95.35 1.47 1 -7 0 91.34 1.45 -1 -7 0 93.10 1.47 1 -7 0 93.22 1.51 -1 -7 0 91.96 1.46 1 7 0 93.43 1.49 1 7 0 95.32 1.50 1 7 0 98.08 1.49 1 7 0 95.90 1.49 -1 7 0 94.36 1.52 1 7 0 99.12 1.50 -1 7 0 97.06 1.50 -2 -7 0 184.78 2.87 -2 -7 0 187.71 2.83 2 -7 0 185.86 2.84 2 -7 0 182.10 2.93 -2 -7 0 187.22 2.83 2 -7 0 189.19 2.83 2 -7 0 187.64 2.86 2 -7 0 186.36 2.84 -2 -7 0 181.73 2.89 -2 7 0 192.76 2.90 2 7 0 187.80 2.92 2 7 0 190.53 2.90 -2 7 0 190.74 2.94 -2 7 0 191.72 2.92 2 7 0 186.51 2.91 2 7 0 188.55 2.90 3 -7 0 54.83 0.96 3 -7 0 56.09 0.95 -3 -7 0 55.59 0.95 3 -7 0 56.03 0.98 -3 -7 0 57.02 0.93 -3 -7 0 57.32 0.99 -3 -7 0 55.35 1.03 3 -7 0 56.01 0.92 3 7 0 55.29 0.96 -3 7 0 56.45 0.99 3 7 0 55.06 0.96 -3 7 0 56.66 0.95 -3 7 0 54.81 0.99 3 7 0 55.12 0.99 -3 7 0 54.12 1.00 4 -7 0 0.15 0.06 4 -7 0 0.38 0.10 -4 -7 0 0.26 0.13 -4 -7 0 0.21 0.10 -4 -7 0 0.26 0.09 -4 -7 0 0.23 0.11 4 -7 0 0.24 0.09 4 7 0 0.42 0.10 4 7 0 0.21 0.08 4 7 0 0.24 0.08 -4 7 0 0.20 0.10 -4 7 0 0.27 0.10 -4 7 0 0.29 0.10 5 -7 0 35.17 0.76 -5 -7 0 33.99 0.85 -5 -7 0 34.34 0.74 -5 -7 0 33.39 0.81 5 -7 0 35.33 0.74 -5 7 0 35.03 0.81 -5 7 0 36.13 0.82 5 7 0 35.08 0.76 5 7 0 36.12 0.75 -5 7 0 36.07 0.80 5 7 0 36.16 0.81 6 -7 0 13.26 0.45 6 -7 0 13.59 0.46 -6 -7 0 13.44 0.54 -6 -7 0 13.03 0.51 -6 7 0 13.75 0.51 6 7 0 13.90 0.50 6 7 0 14.28 0.45 6 7 0 15.12 0.47 -6 7 0 13.78 0.51 0 -8 0 124.73 1.91 0 -8 0 122.97 1.95 0 -8 0 128.19 1.93 0 -8 0 125.45 1.96 0 8 0 131.05 2.04 0 8 0 132.32 2.02 1 -8 0 70.31 1.13 1 -8 0 71.17 1.19 -1 -8 0 71.13 1.13 1 -8 0 69.11 1.13 -1 -8 0 71.55 1.09 1 -8 0 68.57 1.14 -1 -8 0 70.37 1.14 1 -8 0 71.61 1.10 -1 -8 0 70.34 1.15 -1 -8 0 71.80 1.15 1 8 0 70.52 1.12 -1 8 0 70.79 1.15 -1 8 0 69.11 1.17 1 8 0 69.94 1.13 -1 8 0 70.50 1.13 1 8 0 71.95 1.13 -2 -8 0 58.08 0.95 -2 -8 0 56.45 1.00 2 -8 0 56.28 0.97 2 -8 0 56.36 0.95 -2 -8 0 57.44 0.98 -2 -8 0 57.49 0.94 2 -8 0 58.53 0.95 2 -8 0 55.84 1.03 -2 8 0 57.93 0.94 2 8 0 56.15 0.95 -2 8 0 56.83 0.97 2 8 0 56.05 0.96 -2 8 0 56.62 0.99 2 8 0 57.25 0.95 -3 -8 0 28.92 0.53 3 -8 0 27.78 0.56 -3 -8 0 28.97 0.55 3 -8 0 28.81 0.58 -3 -8 0 28.70 0.59 -3 -8 0 27.80 0.62 3 -8 0 28.41 0.55 3 -8 0 28.83 0.52 -3 8 0 29.68 0.61 3 8 0 28.61 0.58 -3 8 0 30.35 0.60 3 8 0 30.08 0.61 -3 8 0 29.48 0.62 3 8 0 29.49 0.58 -4 -8 0 32.23 0.68 4 -8 0 32.02 0.66 -4 -8 0 31.56 0.73 -4 -8 0 32.33 0.76 4 -8 0 32.59 0.62 4 -8 0 31.89 0.67 4 8 0 32.96 0.68 -4 8 0 34.31 0.72 -4 8 0 34.28 0.73 4 8 0 33.02 0.72 4 8 0 33.26 0.67 -4 8 0 33.38 0.73 5 -8 0 7.66 0.31 -5 -8 0 7.59 0.31 -5 -8 0 7.49 0.35 5 -8 0 8.35 0.32 -5 -8 0 7.42 0.37 -5 8 0 7.99 0.34 5 8 0 7.84 0.29 5 8 0 7.76 0.33 -5 8 0 7.88 0.34 -5 8 0 8.09 0.35 5 8 0 7.84 0.31 -6 -8 0 32.67 0.90 6 -8 0 33.29 0.79 6 -8 0 32.80 0.77 -6 -8 0 33.69 0.87 6 8 0 33.10 0.78 -6 8 0 33.16 0.83 6 8 0 33.54 0.83 6 8 0 33.70 0.76 -6 8 0 31.93 0.83 0 -9 0 0.22 0.06 0 -9 0 0.25 0.06 0 -9 0 0.14 0.05 0 9 0 0.14 0.06 0 9 0 0.27 0.06 1 -9 0 72.74 1.17 -1 -9 0 71.42 1.18 -1 -9 0 71.00 1.17 -1 -9 0 72.12 1.11 1 -9 0 71.66 1.22 1 -9 0 70.54 1.17 -1 -9 0 73.18 1.16 1 -9 0 72.89 1.13 1 -9 0 70.64 1.15 -1 -9 0 72.26 1.17 1 9 0 71.98 1.18 1 9 0 74.21 1.17 -1 9 0 72.75 1.22 -1 9 0 72.51 1.18 -1 9 0 72.46 1.20 1 9 0 73.36 1.16 2 -9 0 73.03 1.22 -2 -9 0 73.20 1.25 -2 -9 0 74.27 1.19 -2 -9 0 75.06 1.20 2 -9 0 72.96 1.29 2 -9 0 72.58 1.13 2 -9 0 72.31 1.19 2 -9 0 72.63 1.19 -2 -9 0 72.21 1.23 -2 9 0 71.06 1.15 -2 9 0 71.40 1.18 2 9 0 71.52 1.17 2 9 0 69.80 1.16 2 9 0 70.74 1.17 -2 9 0 70.16 1.20 -3 -9 0 28.26 0.63 -3 -9 0 29.48 0.56 3 -9 0 28.39 0.59 3 -9 0 28.62 0.56 3 -9 0 29.86 0.55 -3 -9 0 28.99 0.61 -3 -9 0 30.15 0.56 3 9 0 29.03 0.57 3 9 0 28.18 0.59 3 9 0 28.69 0.57 -3 9 0 27.70 0.61 -3 9 0 28.04 0.57 -3 9 0 28.07 0.59 -4 -9 0 7.64 0.32 4 -9 0 7.08 0.28 4 -9 0 6.70 0.27 -4 -9 0 7.24 0.28 -4 -9 0 6.77 0.32 4 -9 0 7.42 0.24 -4 9 0 6.54 0.28 -4 9 0 7.18 0.29 -4 9 0 6.90 0.28 4 9 0 6.76 0.26 4 9 0 7.01 0.28 4 9 0 6.98 0.26 5 -9 0 1.36 0.15 -5 -9 0 1.48 0.21 -5 -9 0 1.42 0.19 5 -9 0 1.21 0.16 5 -9 0 1.46 0.17 -5 -9 0 1.50 0.18 5 9 0 1.57 0.16 -5 9 0 2.06 0.21 -5 9 0 2.03 0.29 -5 9 0 1.74 0.20 5 9 0 1.85 0.18 5 9 0 1.51 0.19 -6 -9 0 14.06 0.57 6 -9 0 14.48 0.48 6 -9 0 13.89 0.48 -6 -9 0 13.24 0.53 6 9 0 14.25 0.51 6 9 0 14.37 0.47 6 9 0 14.92 0.46 -6 9 0 13.88 0.51 -6 9 0 14.23 0.62 0 -10 0 67.91 1.16 0 -10 0 76.76 1.15 0 -10 0 69.09 1.12 0 -10 0 69.97 1.14 0 -10 0 69.68 1.18 0 10 0 69.00 1.13 0 10 0 71.07 1.17 -1 -10 0 81.40 1.34 1 -10 0 82.31 1.34 -1 -10 0 81.89 1.35 -1 -10 0 82.29 1.28 1 -10 0 82.99 1.40 1 -10 0 80.63 1.34 1 -10 0 82.63 1.29 -1 -10 0 84.67 1.34 -1 -10 0 83.07 1.33 1 -10 0 82.12 1.32 1 10 0 85.21 1.36 -1 10 0 86.95 1.37 -1 10 0 84.80 1.41 -1 10 0 83.32 1.39 1 10 0 84.30 1.37 1 10 0 84.99 1.34 2 -10 0 138.56 2.17 2 -10 0 133.88 2.18 2 -10 0 139.86 2.28 -2 -10 0 141.43 2.18 -2 -10 0 138.93 2.22 -2 -10 0 140.71 2.16 -2 -10 0 135.46 2.20 2 -10 0 138.84 2.10 2 -10 0 138.20 2.17 -2 10 0 136.98 2.24 -2 10 0 140.09 2.21 2 10 0 140.55 2.20 -2 10 0 142.30 2.17 2 10 0 143.95 2.20 2 10 0 137.04 2.19 -3 -10 0 114.81 1.89 -3 -10 0 116.49 1.83 -3 -10 0 112.91 1.93 3 -10 0 115.65 1.84 3 -10 0 112.75 1.88 3 -10 0 114.98 1.82 -3 -10 0 115.28 1.83 3 10 0 111.22 1.85 -3 10 0 113.89 1.83 3 10 0 113.55 1.83 -3 10 0 114.74 1.89 3 10 0 112.39 1.83 -3 10 0 111.55 1.86 -4 -10 0 22.50 0.59 -4 -10 0 22.43 0.55 4 -10 0 22.85 0.54 4 -10 0 22.58 0.49 -4 -10 0 22.45 0.61 4 10 0 21.73 0.51 -4 10 0 22.88 0.54 4 10 0 23.94 0.53 -4 10 0 22.47 0.57 4 10 0 21.77 0.55 -4 10 0 22.63 0.56 -5 -10 0 27.41 0.75 -5 -10 0 28.12 0.67 -5 -10 0 27.96 0.73 5 -10 0 27.91 0.59 5 -10 0 27.06 0.66 5 10 0 27.98 0.70 -5 10 0 28.08 0.70 -5 10 0 28.01 0.70 5 10 0 28.56 0.64 5 10 0 27.52 0.65 6 -10 0 10.41 0.42 -6 -10 0 10.84 0.49 -6 -10 0 9.90 0.48 6 10 0 10.04 0.43 -6 10 0 10.70 0.46 6 10 0 9.85 0.40 6 10 0 10.38 0.41 0 -11 0 0.39 0.07 0 -11 0 0.27 0.06 0 -11 0 0.33 0.07 -1 -11 0 8.57 0.19 1 -11 0 8.23 0.23 1 -11 0 8.42 0.22 -1 -11 0 8.52 0.25 -1 -11 0 8.30 0.25 1 -11 0 7.64 0.24 1 -11 0 8.41 0.27 1 -11 0 8.20 0.21 -1 -11 0 8.22 0.23 -1 -11 0 8.89 0.24 -1 11 0 7.49 0.23 1 11 0 7.24 0.21 -1 11 0 7.80 0.26 -1 11 0 7.64 0.23 1 11 0 7.71 0.19 1 11 0 7.79 0.23 2 -11 0 129.79 2.06 -2 -11 0 130.31 2.11 2 -11 0 129.56 2.06 2 -11 0 130.77 1.99 -2 -11 0 131.98 2.05 2 -11 0 128.04 2.17 -2 -11 0 130.68 2.10 -2 -11 0 131.68 2.07 2 -11 0 130.89 2.08 -2 11 0 126.47 2.09 -2 11 0 131.21 2.01 2 11 0 127.37 2.05 -2 11 0 130.07 2.06 2 11 0 131.07 2.06 2 11 0 131.02 2.05 3 -11 0 23.63 0.50 -3 -11 0 23.16 0.54 3 -11 0 23.79 0.49 -3 -11 0 23.83 0.49 -3 -11 0 23.08 0.56 3 -11 0 22.93 0.52 3 -11 0 23.90 0.60 3 11 0 24.02 0.53 -3 11 0 24.26 0.54 3 11 0 23.88 0.51 -3 11 0 23.95 0.50 3 11 0 23.84 0.51 -3 11 0 23.88 0.56 4 -11 0 9.77 0.33 -4 -11 0 10.01 0.38 -4 -11 0 9.61 0.37 -4 -11 0 9.60 0.35 4 -11 0 9.63 0.29 -4 11 0 10.41 0.36 4 11 0 10.70 0.36 4 11 0 9.48 0.32 4 11 0 10.10 0.32 -4 11 0 10.26 0.36 5 -11 0 62.60 1.22 5 -11 0 64.86 1.14 -5 -11 0 62.84 1.30 -5 -11 0 60.40 1.31 -5 -11 0 63.74 1.22 5 11 0 64.95 1.28 -5 11 0 65.41 1.28 5 11 0 66.53 1.23 5 11 0 64.08 1.21 0 -12 0 55.51 0.89 0 -12 0 55.39 0.94 0 -12 0 55.13 0.98 0 -12 0 54.10 0.91 0 -12 0 54.27 0.96 0 12 0 54.49 0.96 0 12 0 55.11 0.87 0 12 0 54.92 0.93 1 -12 0 6.03 0.18 -1 -12 0 5.98 0.22 1 -12 0 5.66 0.23 -1 -12 0 6.03 0.16 -1 -12 0 6.14 0.20 -1 -12 0 6.04 0.20 1 -12 0 6.00 0.19 1 -12 0 6.46 0.21 1 -12 0 5.92 0.21 -1 -12 0 6.03 0.22 1 12 0 7.03 0.18 1 12 0 6.01 0.21 -1 12 0 6.29 0.24 -1 12 0 5.92 0.22 -1 12 0 6.01 0.21 1 12 0 6.05 0.19 -2 -12 0 27.32 0.58 -2 -12 0 27.36 0.53 2 -12 0 26.26 0.54 -2 -12 0 26.62 0.55 2 -12 0 25.38 0.61 2 -12 0 27.00 0.55 2 -12 0 28.29 0.57 2 -12 0 26.19 0.53 -2 -12 0 27.14 0.58 2 12 0 28.05 0.55 2 12 0 27.25 0.54 -2 12 0 26.89 0.61 2 12 0 27.49 0.56 -2 12 0 27.57 0.58 -2 12 0 28.36 0.57 3 -12 0 24.18 0.54 3 -12 0 23.71 0.62 -3 -12 0 23.83 0.56 3 -12 0 24.59 0.51 -3 -12 0 24.12 0.51 3 -12 0 24.11 0.52 -3 -12 0 23.86 0.58 3 12 0 24.97 0.55 -3 12 0 24.85 0.58 3 12 0 24.74 0.53 3 12 0 23.80 0.53 -3 12 0 23.94 0.55 -4 -12 0 24.14 0.60 -4 -12 0 24.12 0.63 4 -12 0 24.77 0.54 4 -12 0 24.81 0.59 -4 -12 0 23.82 0.65 4 12 0 24.85 0.57 4 12 0 25.21 0.61 -4 12 0 25.69 0.62 -4 12 0 25.70 0.63 4 12 0 25.85 0.58 -5 -12 0 5.84 0.35 -5 -12 0 5.56 0.31 5 -12 0 6.32 0.30 5 -12 0 6.03 0.26 -5 -12 0 5.81 0.35 5 12 0 6.11 0.30 -5 12 0 6.35 0.33 5 12 0 5.77 0.27 5 12 0 6.46 0.33 0 -13 0 0.56 0.09 0 13 0 0.67 0.10 1 -13 0 51.80 0.98 -1 -13 0 52.30 0.93 1 -13 0 50.65 0.90 -1 -13 0 53.17 0.93 -1 -13 0 52.80 0.91 -1 -13 0 53.04 0.86 1 -13 0 50.51 0.92 1 -13 0 51.56 0.87 -1 -13 0 51.91 0.93 1 -13 0 51.91 0.93 1 13 0 54.64 0.88 -1 13 0 52.42 0.95 1 13 0 52.20 0.91 -1 13 0 52.44 0.98 -1 13 0 54.10 0.94 1 13 0 52.33 0.94 2 -13 0 35.78 0.70 -2 -13 0 38.32 0.74 -2 -13 0 37.20 0.71 2 -13 0 36.71 0.79 2 -13 0 36.51 0.72 -2 -13 0 36.76 0.69 2 -13 0 36.24 0.69 -2 -13 0 36.95 0.74 -2 13 0 37.99 0.72 2 13 0 37.30 0.71 2 13 0 37.52 0.70 -2 13 0 36.57 0.74 -2 13 0 37.04 0.78 2 13 0 37.26 0.69 3 -13 0 86.88 1.61 3 -13 0 88.27 1.47 -3 -13 0 86.37 1.55 3 -13 0 87.95 1.46 3 -13 0 85.61 1.50 -3 -13 0 89.11 1.47 -3 -13 0 87.17 1.52 3 13 0 87.20 1.48 -3 13 0 88.45 1.50 3 13 0 87.03 1.47 -3 13 0 84.88 1.53 3 13 0 86.23 1.47 4 -13 0 2.68 0.20 -4 -13 0 2.70 0.23 4 -13 0 2.47 0.18 -4 -13 0 2.82 0.23 -4 -13 0 2.65 0.24 4 13 0 2.54 0.20 4 13 0 2.73 0.19 4 13 0 2.32 0.18 -4 13 0 2.63 0.22 -4 13 0 2.56 0.22 -5 -13 0 13.07 0.50 5 -13 0 12.74 0.38 -5 -13 0 12.86 0.45 -5 -13 0 12.67 0.50 5 -13 0 13.50 0.45 5 13 0 13.46 0.46 5 13 0 13.77 0.42 5 13 0 13.54 0.44 -5 13 0 14.07 0.48 0 -14 0 10.07 0.30 0 -14 0 9.26 0.28 0 -14 0 10.10 0.25 0 -14 0 10.77 0.32 0 14 0 9.32 0.29 0 14 0 9.11 0.26 -1 -14 0 7.20 0.25 1 -14 0 6.71 0.21 1 -14 0 7.01 0.27 1 -14 0 6.68 0.25 -1 -14 0 7.26 0.23 -1 -14 0 6.77 0.26 -1 -14 0 6.99 0.24 1 -14 0 6.36 0.23 1 -14 0 6.90 0.21 -1 -14 0 7.12 0.19 1 14 0 6.43 0.24 -1 14 0 6.66 0.25 1 14 0 6.35 0.18 -1 14 0 6.13 0.27 1 14 0 6.67 0.22 -1 14 0 6.69 0.24 -2 -14 0 44.77 0.85 2 -14 0 43.19 0.92 2 -14 0 44.13 0.83 -2 -14 0 44.40 0.86 2 -14 0 44.66 0.82 -2 -14 0 44.19 0.84 -2 -14 0 45.30 0.86 2 -14 0 43.44 0.84 2 14 0 42.79 0.80 -2 14 0 44.23 0.83 2 14 0 44.20 0.82 2 14 0 43.84 0.79 -2 14 0 42.97 0.85 -2 14 0 43.19 0.89 -3 -14 0 28.09 0.65 3 -14 0 28.29 0.60 3 -14 0 28.02 0.63 3 -14 0 28.52 0.60 -3 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0.17 -2 -15 0 1.87 0.17 -2 15 0 1.37 0.17 2 15 0 1.89 0.15 -2 15 0 1.80 0.16 2 15 0 1.50 0.15 2 15 0 1.75 0.13 -2 15 0 1.70 0.16 -3 -15 0 15.80 0.41 3 -15 0 15.02 0.43 -3 -15 0 15.58 0.46 3 -15 0 15.53 0.41 3 -15 0 15.68 0.41 3 -15 0 15.68 0.51 -3 -15 0 15.68 0.45 3 15 0 16.12 0.42 -3 15 0 15.52 0.49 3 15 0 15.82 0.42 3 15 0 15.95 0.42 -3 15 0 15.70 0.44 -3 15 0 15.58 0.46 4 -15 0 5.53 0.28 -4 -15 0 6.19 0.32 -4 -15 0 5.48 0.30 4 -15 0 5.64 0.25 -4 -15 0 5.95 0.32 4 15 0 5.85 0.27 -4 15 0 6.09 0.31 -4 15 0 5.53 0.33 4 15 0 6.19 0.27 4 15 0 6.39 0.29 5 -15 0 1.03 0.18 -5 -15 0 1.37 0.21 -5 -15 0 0.82 0.19 -5 -15 0 0.92 0.20 5 -15 0 0.85 0.14 5 15 0 1.30 0.19 5 15 0 1.14 0.17 -5 15 0 0.88 0.19 0 -16 0 44.62 0.87 0 -16 0 43.16 0.85 0 -16 0 44.69 0.82 0 -16 0 43.50 0.79 0 16 0 44.77 0.82 0 16 0 44.25 0.86 1 -16 0 4.74 0.23 -1 -16 0 5.27 0.24 -1 -16 0 4.29 0.21 -1 -16 0 5.61 0.25 -1 -16 0 5.28 0.17 1 -16 0 5.71 0.26 1 -16 0 4.86 0.20 1 -16 0 4.39 0.21 -1 -16 0 5.60 0.22 1 -16 0 4.59 0.19 -1 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2.45 0.25 -1 -2 7 8.79 0.39 1 -2 -7 8.97 0.44 -1 -2 7 9.64 0.38 -1 -2 7 8.55 0.39 1 -2 -7 9.36 0.39 -1 -2 7 8.84 0.39 -1 2 7 8.76 0.38 -1 2 7 8.66 0.39 -1 2 7 9.26 0.36 1 2 -7 8.60 0.39 -1 2 7 9.53 0.40 1 2 -7 9.26 0.45 -4 -3 7 2.99 0.29 4 -3 -7 3.09 0.26 -4 -3 7 2.81 0.27 -4 3 7 3.48 0.33 4 3 -7 3.01 0.25 -4 3 7 2.85 0.27 -3 -3 7 2.57 0.22 3 -3 -7 2.23 0.23 3 -3 -7 2.15 0.22 -3 -3 7 2.23 0.23 -3 -3 7 2.08 0.19 -3 -3 7 2.25 0.24 3 3 -7 2.45 0.23 3 3 -7 3.01 0.27 -3 3 7 2.84 0.28 -3 3 7 2.41 0.24 -2 -3 7 4.77 0.27 2 -3 -7 5.09 0.33 -2 -3 7 4.92 0.30 -2 -3 7 4.71 0.28 2 -3 -7 4.05 0.28 -2 -3 7 4.17 0.31 -2 3 7 4.19 0.28 -2 3 7 4.67 0.26 2 3 -7 4.39 0.33 -2 3 7 4.05 0.29 2 3 -7 4.29 0.30 1 -3 -7 0.74 0.16 -1 -3 7 0.41 0.14 1 -3 -7 0.25 0.15 -1 -3 7 0.42 0.14 -1 -3 7 0.67 0.16 1 3 -7 0.37 0.15 -1 3 7 0.40 0.14 1 3 -7 0.35 0.16 -1 3 7 0.42 0.15 -1 3 7 0.31 0.13 -4 -4 7 8.44 0.41 4 -4 -7 8.98 0.38 -4 -4 7 8.48 0.41 4 4 -7 9.13 0.37 -4 4 7 8.64 0.45 -4 4 7 9.01 0.39 3 -4 -7 17.59 0.55 3 -4 -7 18.04 0.54 -3 -4 7 19.05 0.52 -3 -4 7 17.84 0.50 -3 -4 7 17.49 0.56 3 4 -7 16.92 0.55 -3 4 7 17.99 0.54 -3 4 7 16.96 0.59 3 4 -7 17.05 0.52 -2 -4 7 11.85 0.41 2 -4 -7 11.50 0.47 2 -4 -7 11.86 0.43 -2 -4 7 12.17 0.43 -2 -4 7 11.52 0.45 2 4 -7 10.63 0.46 -2 4 7 11.34 0.39 -2 4 7 11.12 0.42 2 4 -7 11.10 0.43 -2 4 7 11.29 0.46 -1 -4 7 9.06 0.37 1 -4 -7 9.07 0.44 -1 -4 7 8.64 0.39 -1 -4 7 8.79 0.38 1 -4 -7 8.65 0.38 1 4 -7 8.41 0.39 1 4 -7 8.60 0.44 -1 4 7 9.10 0.41 -1 4 7 8.85 0.39 -1 4 7 9.48 0.37 -3 -5 7 2.45 0.22 3 -5 -7 2.62 0.25 -3 -5 7 2.60 0.23 3 -5 -7 2.85 0.25 -3 -5 7 2.48 0.26 -3 5 7 2.65 0.24 3 5 -7 3.11 0.26 -3 5 7 2.89 0.29 3 5 -7 2.73 0.26 2 -5 -7 15.79 0.54 -2 -5 7 15.69 0.48 2 -5 -7 15.71 0.50 -2 -5 7 14.68 0.50 -2 -5 7 15.87 0.49 -2 5 7 14.81 0.54 2 5 -7 14.45 0.50 2 5 -7 15.41 0.55 -2 5 7 15.33 0.50 -2 5 7 16.00 0.46 1 -5 -7 3.23 0.28 -1 -5 7 2.90 0.27 -1 -5 7 2.83 0.26 -1 -5 7 3.56 0.26 1 -5 -7 2.42 0.26 1 -5 -7 3.12 0.27 -1 5 7 3.25 0.25 1 5 -7 2.98 0.26 -1 5 7 3.57 0.26 1 5 -7 3.08 0.30 -1 5 7 3.48 0.29 -3 -6 7 9.85 0.38 -3 -6 7 10.42 0.39 -3 -6 7 9.62 0.42 3 -6 -7 10.64 0.41 3 -6 -7 10.28 0.43 -3 6 7 9.96 0.46 3 6 -7 10.40 0.44 3 6 -7 10.86 0.42 -3 6 7 10.46 0.41 -2 -6 7 0.30 0.13 -2 -6 7 0.24 0.14 2 -6 -7 0.20 0.14 2 -6 -7 0.56 0.15 2 -6 -7 0.27 0.15 -2 -6 7 0.41 0.13 -2 6 7 0.17 0.13 2 6 -7 0.50 0.16 2 6 -7 0.18 0.15 -2 6 7 0.21 0.12 -2 6 7 0.39 0.15 -1 -6 7 3.55 0.28 1 -6 -7 3.59 0.30 1 -6 -7 3.63 0.32 1 -6 -7 3.60 0.30 -1 -6 7 3.22 0.27 -1 -6 7 3.61 0.27 -1 6 7 4.19 0.27 1 6 -7 3.38 0.32 -1 6 7 4.55 0.30 1 6 -7 4.24 0.30 -1 6 7 3.89 0.30 -3 -7 7 9.67 0.43 3 -7 -7 9.75 0.40 -3 -7 7 9.49 0.38 -3 -7 7 11.24 0.43 3 -7 -7 9.86 0.42 -3 7 7 9.58 0.39 3 7 -7 9.55 0.40 -3 7 7 9.68 0.46 3 7 -7 10.27 0.44 2 -7 -7 2.59 0.24 -2 -7 7 2.33 0.22 -2 -7 7 2.47 0.25 2 -7 -7 2.19 0.25 2 -7 -7 2.28 0.23 -2 -7 7 2.52 0.24 2 7 -7 2.47 0.26 2 7 -7 2.31 0.24 -2 7 7 2.39 0.20 -2 7 7 2.53 0.24 -2 7 7 2.59 0.27 -2 -8 7 3.50 0.28 -2 -8 7 3.64 0.28 -2 -8 7 3.78 0.27 2 -8 -7 3.18 0.30 2 -8 -7 3.62 0.29 -2 8 7 3.85 0.32 2 8 -7 3.86 0.32 2 8 -7 3.67 0.29 -2 8 7 3.82 0.28 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 58013 _shelx_res_file ; TITL s1 in P21 #4 chiral.res created by SHELXL-2017/1 at 11:20:05 on 11-Jun-2019 REM reset to P21 #4 CELL 0.71073 4.8838 18.3867 5.1522 90 110.3246 90 ZERR 2 0.0002 0.0007 0.0002 0 0.0016 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 12 22 2 12 2 L.S. 12 0 0 PLAN 20 SIZE 0.02 0.28 0.45 TEMP -173.15 BOND fmap 2 53 ACTA REM REM REM WGHT 0.033300 0.060900 FVAR 0.41848 S1 5 0.854113 0.894959 0.848093 11.00000 0.00737 0.00812 = 0.01511 0.00364 0.00073 -0.00088 O6 4 0.121951 0.691754 0.523041 11.00000 0.01359 0.01266 = 0.01575 -0.00395 0.00676 -0.00612 H6 2 0.005631 0.664478 0.560725 11.00000 -1.50000 O4 4 1.046245 0.928634 1.096529 11.00000 0.02063 0.01664 = 0.02080 0.00447 -0.01003 -0.00828 O5 4 0.253731 0.722080 0.971069 11.00000 0.01845 0.01095 = 0.01521 0.00056 0.00746 -0.00321 C1 1 0.439350 1.067704 0.392768 11.00000 0.00775 0.00706 = 0.00956 0.00093 0.00171 -0.00065 C6 1 0.281335 0.728133 0.747448 11.00000 0.00972 0.00643 = 0.01432 -0.00054 0.00471 0.00002 O2 4 0.265705 1.098308 0.487281 11.00000 0.01300 0.01642 = 0.01302 0.00159 0.00465 0.00723 N1 3 0.814327 1.075749 0.857916 11.00000 0.00877 0.00859 = 0.00878 -0.00065 0.00150 -0.00039 H1A 2 0.997962 1.065258 0.950815 11.00000 -1.50000 H1B 2 0.800543 1.120963 0.816460 11.00000 -1.50000 H1C 2 0.707227 1.072647 0.956772 11.00000 -1.50000 O1 4 0.418004 1.063284 0.144945 11.00000 0.01058 0.01798 = 0.00788 0.00124 0.00250 -0.00080 C4 1 0.669709 0.821848 0.938685 11.00000 0.01175 0.00877 = 0.01291 0.00248 0.00278 -0.00239 H4A 2 0.817983 0.795420 1.062907 11.00000 -1.20000 H4B 2 0.547593 0.842960 1.022603 11.00000 -1.20000 C3 1 0.573011 0.957923 0.679056 11.00000 0.00742 0.00708 = 0.01223 0.00080 0.00106 -0.00007 C2 1 0.696497 1.028586 0.608046 11.00000 0.00786 0.00661 = 0.00769 0.00001 0.00188 0.00018 H2 2 0.853768 1.021164 0.541018 11.00000 -1.20000 O3 4 0.980326 0.870270 0.648409 11.00000 0.01863 0.01426 = 0.03563 0.00592 0.01770 0.00353 C5 1 0.497455 0.777385 0.686736 11.00000 0.01194 0.00930 = 0.01573 -0.00158 0.00721 -0.00247 H5A 2 0.395335 0.806796 0.532521 11.00000 -1.20000 H5B 2 0.617858 0.747118 0.621006 11.00000 -1.20000 H3A 2 0.445457 0.934572 0.516687 11.00000 -1.20000 H3B 2 0.459386 0.966366 0.796806 11.00000 -1.20000 HKLF 4 REM s1 in P21 #4 REM R1 = 0.0189 for 2644 Fo > 4sig(Fo) and 0.0190 for all 2656 data REM 160 parameters refined using 1 restraints END WGHT 0.0329 0.0628 REM Highest difference peak 0.314, deepest hole -0.179, 1-sigma level 0.048 Q1 1 1.0103 0.8813 0.7750 11.00000 0.05 0.31 Q2 1 0.5623 1.0480 0.5005 11.00000 0.05 0.30 Q3 1 0.8973 0.9133 0.9758 11.00000 0.05 0.30 Q4 1 0.7729 0.8583 0.8803 11.00000 0.05 0.27 Q5 1 0.4137 1.0603 0.2607 11.00000 0.05 0.25 Q6 1 0.6338 0.9951 0.6451 11.00000 0.05 0.25 Q7 1 0.9642 0.9427 1.1706 11.00000 0.05 0.25 Q8 1 0.7135 0.9267 0.7651 11.00000 0.05 0.23 Q9 1 0.5944 0.8021 0.8168 11.00000 0.05 0.22 Q10 1 0.7419 1.0530 0.7370 11.00000 0.05 0.22 Q11 1 0.3784 0.7553 0.7196 11.00000 0.05 0.21 Q12 1 0.1710 0.7128 0.6218 11.00000 0.05 0.19 Q13 1 0.2862 1.0586 0.0540 11.00000 0.05 0.16 Q14 1 0.3054 1.1382 0.4847 11.00000 0.05 0.15 Q15 1 0.1624 0.6829 0.4338 11.00000 0.05 0.15 Q16 1 0.1351 1.1026 0.3985 11.00000 0.05 0.14 Q17 1 0.1553 0.6977 0.9673 11.00000 0.05 0.14 Q18 1 0.0458 0.7195 0.4723 11.00000 0.05 0.14 Q19 1 0.4252 0.7144 1.0956 11.00000 0.05 0.13 Q20 1 0.4000 1.0974 0.0970 11.00000 0.05 0.13 ; _shelx_res_checksum 67125 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S1 0.85411(6) 0.89496(2) 0.84809(6) 0.01103(8) Uani d 1 . . O O6 0.1220(2) 0.69175(6) 0.5230(2) 0.01356(19) Uani d 1 . . H H6 0.006(6) 0.6645(14) 0.561(5) 0.020 Uiso d 1 . . O O4 1.0462(3) 0.92863(7) 1.0965(3) 0.0239(3) Uani d 1 . . O O5 0.2537(2) 0.72208(6) 0.9711(2) 0.0144(2) Uani d 1 . . C C1 0.4393(3) 1.06770(7) 0.3928(3) 0.0085(2) Uani d 1 . . C C6 0.2813(3) 0.72813(7) 0.7474(3) 0.0100(2) Uani d 1 . . O O2 0.2657(2) 1.09831(6) 0.4873(2) 0.0141(2) Uani d 1 . . N N1 0.8143(3) 1.07575(6) 0.8579(2) 0.0091(2) Uani d 1 . . H H1A 0.998(5) 1.0653(13) 0.951(5) 0.014 Uiso d 1 . . H H1B 0.801(5) 1.1210(14) 0.816(4) 0.014 Uiso d 1 . . H H1C 0.707(5) 1.0726(13) 0.957(5) 0.014 Uiso d 1 . . O O1 0.4180(2) 1.06328(6) 0.14494(19) 0.01234(18) Uani d 1 . . C C4 0.6697(3) 0.82185(7) 0.9387(3) 0.0115(2) Uani d 1 . . H H4A 0.818(5) 0.7954(13) 1.063(4) 0.014 Uiso d 1 . . H H4B 0.548(5) 0.8430(13) 1.023(4) 0.014 Uiso d 1 . . C C3 0.5730(3) 0.95792(7) 0.6791(3) 0.0095(2) Uani d 1 . . C C2 0.6965(3) 1.02859(7) 0.6080(2) 0.0076(2) Uani d 1 . . H H2 0.854(5) 1.0212(12) 0.541(4) 0.009 Uiso d 1 . . O O3 0.9803(3) 0.87027(6) 0.6484(3) 0.0207(2) Uani d 1 . . C C5 0.4975(3) 0.77739(7) 0.6867(3) 0.0117(2) Uani d 1 . . H H5A 0.395(5) 0.8068(13) 0.533(4) 0.014 Uiso d 1 . . H H5B 0.618(5) 0.7471(14) 0.621(4) 0.014 Uiso d 1 . . H H3A 0.445(5) 0.9346(13) 0.517(5) 0.014 Uiso d 1 . . H H3B 0.459(5) 0.9664(12) 0.797(5) 0.014 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 0.00737(13) 0.00812(13) 0.01511(13) -0.00088(11) 0.00073(9) 0.00364(11) O6 0.0136(4) 0.0127(4) 0.0158(4) -0.0061(4) 0.0068(4) -0.0039(3) O4 0.0206(6) 0.0166(5) 0.0208(5) -0.0083(4) -0.0100(4) 0.0045(4) O5 0.0184(5) 0.0110(5) 0.0152(4) -0.0032(4) 0.0075(4) 0.0006(3) C1 0.0077(5) 0.0071(5) 0.0096(5) -0.0006(4) 0.0017(4) 0.0009(4) C6 0.0097(5) 0.0064(5) 0.0143(5) 0.0000(4) 0.0047(4) -0.0005(4) O2 0.0130(5) 0.0164(5) 0.0130(4) 0.0072(4) 0.0046(4) 0.0016(4) N1 0.0088(5) 0.0086(5) 0.0088(4) -0.0004(4) 0.0015(4) -0.0006(3) O1 0.0106(4) 0.0180(5) 0.0079(4) -0.0008(4) 0.0025(3) 0.0012(4) C4 0.0118(6) 0.0088(5) 0.0129(5) -0.0024(4) 0.0028(4) 0.0025(4) C3 0.0074(5) 0.0071(5) 0.0122(5) -0.0001(4) 0.0011(4) 0.0008(4) C2 0.0079(5) 0.0066(5) 0.0077(4) 0.0002(4) 0.0019(4) 0.0000(4) O3 0.0186(5) 0.0143(5) 0.0356(6) 0.0035(4) 0.0177(5) 0.0059(4) C5 0.0119(5) 0.0093(5) 0.0157(5) -0.0025(5) 0.0072(4) -0.0016(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O4 S1 C4 . . 109.09(7) ? O4 S1 C3 . . 108.07(7) ? O4 S1 O3 . . 117.48(9) ? C4 S1 C3 . . 104.31(6) ? O3 S1 C4 . . 109.37(7) ? O3 S1 C3 . . 107.71(7) ? O2 C1 C2 . . 115.16(11) ? O1 C1 O2 . . 127.01(13) ? O1 C1 C2 . . 117.75(12) ? O6 C6 C5 . . 111.32(11) ? O5 C6 O6 . . 123.82(13) ? O5 C6 C5 . . 124.85(12) ? C5 C4 S1 . . 111.44(9) ? C2 C3 S1 . . 111.67(9) ? N1 C2 C1 . . 108.94(10) ? N1 C2 C3 . . 110.69(10) ? C3 C2 C1 . . 106.21(10) ? C6 C5 C4 . . 111.54(11) ? C6 O6 H6 . . 109.9(17) ? C2 N1 H1A . . 111.0(16) ? C2 N1 H1B . . 112.0(13) ? C2 N1 H1C . . 110.2(16) ? H1A N1 H1B . . 109(2) ? H1A N1 H1C . . 113(2) ? H1B N1 H1C . . 102(2) ? N1 C2 H2 . . 106.1(13) ? C1 C2 H2 . . 111.4(12) ? C3 C2 H2 . . 113.5(13) ? S1 C3 H3A . . 107.2(15) ? S1 C3 H3B . . 108.2(14) ? C2 C3 H3A . . 111.4(15) ? C2 C3 H3B . . 112.0(13) ? H3A C3 H3B . . 106(2) ? S1 C4 H4A . . 103.6(15) ? S1 C4 H4B . . 105.7(15) ? C5 C4 H4A . . 112.3(14) ? C5 C4 H4B . . 111.7(14) ? H4A C4 H4B . . 111.7(19) ? C4 C5 H5A . . 112.5(14) ? C4 C5 H5B . . 113.0(14) ? C6 C5 H5A . . 108.2(15) ? C6 C5 H5B . . 106.7(15) ? H5A C5 H5B . . 104.4(19) ? 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 O4 . 1.4380(12) ? S1 C4 . 1.7686(13) ? S1 C3 . 1.7756(13) ? S1 O3 . 1.4440(12) ? O6 C6 . 1.3285(16) ? O5 C6 . 1.2107(16) ? C1 O2 . 1.2489(16) ? C1 O1 . 1.2471(15) ? C1 C2 . 1.5353(18) ? C6 C5 . 1.5038(19) ? N1 C2 . 1.4919(16) ? C4 C5 . 1.5174(19) ? C3 C2 . 1.5293(18) ? O6 H6 . 0.83(3) ? N1 H1A . 0.88(3) ? N1 H1B . 0.86(3) ? N1 H1C . 0.85(3) ? C2 H2 . 0.96(2) ? C3 H3A . 0.95(2) ? C3 H3B . 0.97(3) ? C4 H4A . 0.92(2) ? C4 H4B . 0.93(2) ? C5 H5A . 0.95(2) ? C5 H5B . 0.95(2) ? 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 N1 H1A O1 1_656 0.88(3) 1.95(3) 2.8113(17) 168(2) yes N1 H1A O4 . 0.88(3) 2.61(2) 3.0239(17) 109.9(19) yes N1 H1B O5 2_657 0.86(3) 2.22(2) 2.8860(16) 134.4(18) yes N1 H1B O6 2_656 0.86(3) 2.31(2) 2.9869(15) 136.0(19) yes N1 H1C O1 1_556 0.85(3) 1.98(3) 2.8238(17) 173(2) yes O6 H6 O2 2_546 0.83(3) 1.75(3) 2.5436(15) 159(2) 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 O3 S1 C3 C2 . . . . -69.00(11) ? O4 S1 C3 C2 . . . . 58.88(12) ? C4 S1 C3 C2 . . . . 174.85(9) ? O3 S1 C4 C5 . . . . -41.94(13) ? O4 S1 C4 C5 . . . . -171.68(11) ? C3 S1 C4 C5 . . . . 73.05(11) ? O1 C1 C2 N1 . . . . 139.90(13) ? O1 C1 C2 C3 . . . . -100.88(14) ? O2 C1 C2 N1 . . . . -43.00(16) ? O2 C1 C2 C3 . . . . 76.23(14) ? N1 C2 C3 S1 . . . . -78.37(13) ? C1 C2 C3 S1 . . . . 163.54(9) ? S1 C4 C5 C6 . . . . -165.17(10) ? C4 C5 C6 O5 . . . . -2.7(2) ? C4 C5 C6 O6 . . . . 177.18(12) ? O3 S1 C3 H3A . . . . 53.3(16) ? O3 S1 C3 H3B . . . . 167.4(15) ? O4 S1 C3 H3A . . . . -178.8(16) ? O4 S1 C3 H3B . . . . -64.8(15) ? C4 S1 C3 H3A . . . . -62.8(16) ? C4 S1 C3 H3B . . . . 51.2(15) ? O3 S1 C4 H4A . . . . 79.0(14) ? O3 S1 C4 H4B . . . . -163.4(13) ? O4 S1 C4 H4A . . . . -50.8(14) ? O4 S1 C4 H4B . . . . 66.8(13) ? C3 S1 C4 H4A . . . . -166.1(14) ? C3 S1 C4 H4B . . . . -48.4(13) ? H6 O6 C6 O5 . . . . -1(2) ? H6 O6 C6 C5 . . . . 179(2) ? O1 C1 C2 H2 . . . . 23.2(14) ? O2 C1 C2 H2 . . . . -159.7(14) ? C1 C2 N1 H1A . . . . -155.6(17) ? C1 C2 N1 H1B . . . . -33.7(18) ? C1 C2 N1 H1C . . . . 79.2(18) ? C3 C2 N1 H1A . . . . 88.0(17) ? C3 C2 N1 H1B . . . . -150.1(18) ? C3 C2 N1 H1C . . . . -37.2(18) ? H2 C2 N1 H1A . . . . -36(2) ? H2 C2 N1 H1B . . . . 86(2) ? H2 C2 N1 H1C . . . . -161(2) ? N1 C2 C3 H3A . . . . 161.7(17) ? N1 C2 C3 H3B . . . . 43.1(16) ? C1 C2 C3 H3A . . . . 43.7(17) ? C1 C2 C3 H3B . . . . -75.0(16) ? H2 C2 C3 S1 . . . . 40.8(13) ? H2 C2 C3 H3A . . . . -79(2) ? H2 C2 C3 H3B . . . . 162(2) ? S1 C4 C5 H5A . . . . -43.3(17) ? S1 C4 C5 H5B . . . . 74.7(16) ? H4A C4 C5 C6 . . . . 79.1(16) ? H4A C4 C5 H5A . . . . -159(2) ? H4A C4 C5 H5B . . . . -41(2) ? H4B C4 C5 C6 . . . . -47.2(15) ? H4B C4 C5 H5A . . . . 75(2) ? H4B C4 C5 H5B . . . . -167(2) ? H5A C5 C6 O5 . . . . -127.0(14) ? H5A C5 C6 O6 . . . . 52.9(14) ? H5B C5 C6 O5 . . . . 121.2(13) ? H5B C5 C6 O6 . . . . -59.0(13) ?