#------------------------------------------------------------------------------ #$Date: 2019-05-15 08:10:51 +0300 (Wed, 15 May 2019) $ #$Revision: 215178 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/10/1551061.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_1551061 loop_ _publ_author_name 'Toure, Assane' 'Diop, Cheikh Abdoul Khadir' 'Diop, Libasse' 'Plasseraud, Laurent' 'Cattey, H\'el\`ene' _publ_section_title ; Ethylammonium hydrogen oxalate--oxalic acid (2/1) ; _journal_coeditor_code BV4024 _journal_issue 5 _journal_name_full IUCrData _journal_page_first x190635 _journal_paper_doi 10.1107/S2414314619006357 _journal_volume 4 _journal_year 2019 _chemical_formula_iupac 'C2 H8 N +, C2 H O4 -, 0.5C2 H2 O4' _chemical_formula_moiety '2(C2 H8 N +), 2(C2 H O4 -), C2 H2 O4' _chemical_formula_sum 'C10 H20 N2 O12' _chemical_formula_weight 360.28 _chemical_name_systematic ; Ethylammonium hydrogen oxalate--oxalic acid (2/1) ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 91.509(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.1667(8) _cell_length_b 6.6243(3) _cell_length_c 11.3247(4) _cell_measurement_reflns_used 7758 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.494 _cell_measurement_theta_min 3.223 _cell_volume 1587.34(11) _computing_cell_refinement ; SAINT (Bruker, 2014) ; _computing_data_collection ; APEX3 (Bruker, 2014) ; _computing_data_reduction ; SAINT (Bruker, 2014) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100 _diffrn_detector CMOS _diffrn_detector_area_resol_mean '1024 x 1024' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device '\k-geometry diffractometer triump Mo' _diffrn_measurement_device_type 'Bruker D8 Venture triumph Mo' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'TRIUMPH curved crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_unetI/netI 0.0146 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 14201 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.531 _diffrn_reflns_theta_min 3.222 _diffrn_source 'X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.7117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2014) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.508 _exptl_crystal_description prism _exptl_crystal_F_000 760 _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.495 _refine_diff_density_min -0.196 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 113 _refine_ls_number_reflns 1829 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0281 _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^)+(0.0383P)^2^+1.1891P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.0747 _reflns_number_gt 1624 _reflns_number_total 1829 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file bv4024sup1.cif _cod_data_source_block I _cod_database_code 1551061 _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 0.937 _shelx_estimated_absorpt_t_max 0.977 _shelx_hkl_file ; -4 0 0 1256.27 28.40 4 0 0 1337.47 28.50 -4 0 0 1262.77 28.40 -6 0 0 2598.04 56.99 6 0 0 2535.05 56.79 6 0 0 2466.65 55.99 -6 0 0 2566.84 56.69 -8 0 0 30.50 1.30 8 0 0 28.20 1.30 8 0 0 29.70 1.30 -8 0 0 29.30 1.30 10 0 0 332.57 8.10 10 0 0 330.67 8.10 -10 0 0 341.47 7.40 -10 0 0 333.47 8.00 -10 0 0 311.17 7.90 -12 0 0 555.34 12.10 12 0 0 529.45 12.90 -12 0 0 549.54 12.80 -12 0 0 538.05 12.80 12 0 0 547.25 12.90 14 0 0 14.90 1.50 -14 0 0 14.60 1.40 14 0 0 12.50 1.50 -14 0 0 15.30 0.60 -14 0 0 15.40 0.50 -14 0 0 16.30 1.40 -16 0 0 141.29 4.30 -16 0 0 148.09 4.30 16 0 0 144.09 4.60 16 0 0 142.79 4.60 -18 0 0 135.59 4.30 18 0 0 132.09 4.60 -18 0 0 134.89 4.30 18 0 0 139.29 4.70 20 0 0 134.09 4.80 -20 0 0 135.19 4.40 20 0 0 111.99 5.60 -20 0 0 132.89 4.30 22 0 0 338.37 9.60 22 0 0 330.57 9.50 -22 0 0 329.47 8.80 -22 0 0 337.37 8.80 -24 0 0 2.50 1.60 -24 0 0 3.20 1.50 24 0 0 3.80 2.00 24 0 0 4.80 2.00 26 0 0 -2.60 2.20 -26 0 0 3.30 1.90 -26 0 0 -2.00 1.60 26 0 0 4.50 2.40 1 -1 0 688.13 15.00 1 -1 0 625.64 15.00 -1 -1 0 687.23 15.00 1 1 0 602.64 14.90 -1 1 0 665.63 15.00 -1 1 0 671.83 15.00 1 1 0 676.73 15.00 1 1 0 692.63 15.00 -3 -1 0 124.59 3.20 3 -1 0 124.69 3.20 -3 -1 0 131.09 3.20 3 -1 0 126.29 3.20 3 -1 0 127.59 3.10 -3 -1 0 128.49 3.20 -3 1 0 125.99 3.20 -3 1 0 119.39 3.10 3 1 0 125.19 3.20 -3 1 0 128.99 3.20 3 1 0 129.29 3.20 -5 -1 0 1652.53 36.60 5 -1 0 1657.33 36.30 5 -1 0 1623.34 36.40 5 -1 0 1655.83 36.30 -5 -1 0 1625.54 36.30 -5 -1 0 1634.34 36.30 5 1 0 1621.24 36.30 -5 1 0 1647.94 36.50 -5 1 0 1589.74 36.20 5 1 0 1608.24 36.30 -5 1 0 1706.83 36.30 7 -1 0 44.30 1.60 7 -1 0 43.20 1.20 -7 -1 0 42.90 1.50 -7 -1 0 45.00 1.60 7 -1 0 41.30 1.60 -7 -1 0 40.30 1.60 -7 1 0 42.50 1.20 7 1 0 42.90 1.60 -7 1 0 42.70 1.50 -7 1 0 41.60 1.50 7 1 0 42.90 1.60 -9 -1 0 62.39 2.10 -9 -1 0 58.29 2.10 -9 -1 0 60.49 1.90 9 -1 0 58.49 2.10 9 -1 0 60.19 2.10 -9 1 0 59.79 1.50 9 1 0 57.89 2.10 -9 1 0 59.29 2.00 -9 1 0 56.69 2.00 9 1 0 59.49 2.20 11 -1 0 70.79 2.50 -11 -1 0 69.79 2.50 11 -1 0 70.39 2.50 -11 -1 0 70.99 2.20 -11 1 0 70.79 2.40 -11 1 0 70.39 2.40 11 1 0 73.69 2.60 11 1 0 73.69 2.60 -13 -1 0 510.05 12.00 -13 -1 0 519.95 11.60 -13 -1 0 492.45 11.90 13 -1 0 495.05 12.10 13 -1 0 480.95 12.00 13 1 0 501.25 12.10 13 1 0 492.75 12.10 -13 1 0 496.85 11.90 -13 1 0 502.85 11.90 -15 -1 0 57.69 2.00 15 -1 0 56.29 2.60 -15 -1 0 56.99 2.40 -15 -1 0 53.39 2.40 15 1 0 54.29 2.60 -15 1 0 59.89 2.40 15 1 0 56.79 2.60 -15 1 0 56.19 2.40 -17 -1 0 169.98 5.00 -17 -1 0 175.38 4.40 -17 -1 0 175.08 5.10 17 -1 0 174.98 5.30 17 -1 0 168.58 5.30 -17 1 0 163.88 4.90 17 1 0 169.98 5.30 17 1 0 162.08 5.20 -17 1 0 166.48 4.90 -19 -1 0 25.20 1.30 -19 -1 0 26.80 2.10 19 -1 0 27.30 2.40 -19 -1 0 23.50 2.10 19 -1 0 23.40 2.70 19 1 0 24.30 2.30 -19 1 0 23.80 2.10 -19 1 0 27.00 2.10 19 1 0 24.40 2.40 -21 -1 0 1269.17 28.70 -21 -1 0 1224.18 28.70 21 -1 0 1216.98 29.20 21 -1 0 1280.17 29.30 -21 -1 0 1239.88 27.40 -21 1 0 1220.58 28.50 -21 1 0 1262.17 28.60 21 1 0 1219.48 29.30 21 1 0 1261.17 29.30 23 -1 0 215.78 7.20 23 -1 0 218.28 7.20 -23 -1 0 211.48 6.50 -23 -1 0 224.08 6.50 -23 1 0 214.48 6.30 23 1 0 214.08 7.20 23 1 0 214.38 7.20 -23 1 0 210.48 6.30 25 -1 0 90.59 5.00 -25 -1 0 88.79 4.20 25 -1 0 73.99 4.90 -25 -1 0 81.89 4.10 -25 1 0 71.49 3.80 25 1 0 90.79 5.10 -25 1 0 87.89 4.00 25 1 0 84.39 5.10 27 -1 0 22.40 3.40 27 -1 0 20.50 3.30 27 1 0 27.10 4.70 27 1 0 28.50 3.70 0 -2 0 9835.22 220.08 0 -2 0 9822.52 220.48 0 -2 0 9801.22 220.08 0 2 0 9934.81 219.98 0 2 0 9999.00 219.98 0 2 0 9992.10 220.58 2 -2 0 4386.96 96.69 -2 -2 0 4182.58 95.19 -2 -2 0 4223.88 96.39 -2 -2 0 4409.96 96.39 2 -2 0 4133.09 95.19 2 -2 0 4361.96 96.89 -2 2 0 4414.26 96.99 -2 2 0 4298.07 96.19 2 2 0 4132.29 95.29 -2 2 0 4474.05 96.89 2 2 0 4401.36 97.19 2 2 0 4185.48 95.69 4 -2 0 1653.33 36.40 4 -2 0 1673.63 36.30 -4 -2 0 1576.44 36.40 -4 -2 0 1589.14 36.50 -4 -2 0 1641.04 36.40 4 -2 0 1610.04 36.40 -4 2 0 1689.43 36.30 -4 2 0 1595.04 36.30 -4 2 0 1570.74 36.30 4 2 0 1687.13 36.40 4 2 0 1680.73 36.50 6 -2 0 474.65 11.00 6 -2 0 449.86 10.90 6 -2 0 441.26 10.70 -6 -2 0 464.75 10.90 -6 -2 0 460.65 10.90 -6 -2 0 449.86 11.00 -6 2 0 462.65 10.90 -6 2 0 479.85 10.70 6 2 0 461.75 11.00 6 2 0 472.45 11.00 -6 2 0 475.85 10.90 8 -2 0 1.20 0.60 -8 -2 0 1.90 0.60 -8 -2 0 1.20 0.60 -8 -2 0 1.80 0.70 8 -2 0 1.00 0.40 8 -2 0 2.30 0.60 -8 2 0 1.60 0.50 -8 2 0 1.90 0.60 8 2 0 1.50 0.60 -8 2 0 1.40 0.60 8 2 0 0.80 0.60 -10 -2 0 79.29 2.70 10 -2 0 79.29 2.70 -10 -2 0 81.49 2.70 -10 -2 0 77.19 2.60 10 -2 0 78.39 2.20 10 -2 0 75.39 2.70 -10 2 0 73.29 2.60 10 2 0 78.59 2.80 -10 2 0 77.99 2.60 -10 2 0 78.09 2.20 10 2 0 77.49 2.80 12 -2 0 280.37 7.30 -12 -2 0 274.77 7.20 -12 -2 0 277.87 7.00 12 -2 0 258.37 7.10 -12 -2 0 276.37 7.20 12 -2 0 278.37 6.50 -12 2 0 284.97 7.10 12 2 0 275.67 7.30 -12 2 0 267.37 7.00 12 2 0 272.87 7.30 14 -2 0 9.20 1.20 -14 -2 0 14.40 1.40 -14 -2 0 12.50 1.40 14 -2 0 13.70 1.50 -14 -2 0 13.60 1.60 -14 2 0 8.90 1.10 14 2 0 13.80 1.70 14 2 0 14.70 1.70 -14 2 0 11.20 1.20 16 -2 0 169.38 5.20 16 -2 0 170.08 5.20 -16 -2 0 160.68 5.00 -16 -2 0 166.28 4.80 16 2 0 166.88 5.30 -16 2 0 165.08 4.90 -16 2 0 158.48 4.80 16 2 0 168.08 5.30 -18 -2 0 33.10 2.30 18 -2 0 30.50 3.60 -18 -2 0 34.00 2.00 -18 -2 0 31.90 2.40 18 -2 0 34.80 2.50 18 2 0 33.80 2.50 18 2 0 33.90 2.60 -18 2 0 32.40 2.30 -18 2 0 33.90 2.20 -20 -2 0 -0.50 0.90 -20 -2 0 -0.50 1.30 20 -2 0 0.90 1.40 -20 -2 0 -0.90 1.20 -20 2 0 0.20 1.20 20 2 0 1.10 1.50 20 2 0 -0.20 1.40 -20 2 0 -2.10 1.20 22 -2 0 -1.00 1.70 -22 -2 0 2.00 1.50 22 -2 0 -1.60 1.60 -22 -2 0 0.60 1.50 -22 -2 0 -0.90 1.00 -22 2 0 -0.90 1.30 -22 2 0 -0.20 1.40 22 2 0 -0.20 1.70 22 2 0 1.70 1.90 -24 -2 0 55.69 4.20 24 -2 0 57.09 4.10 -24 -2 0 60.89 3.70 -24 2 0 57.09 3.50 24 2 0 60.59 4.30 24 2 0 62.79 4.60 -24 2 0 60.49 3.40 26 -2 0 39.20 4.40 -26 -2 0 25.20 4.20 26 -2 0 34.50 3.90 -26 -2 0 30.30 2.90 26 2 0 29.60 3.50 -26 2 0 31.60 3.40 26 2 0 33.40 3.90 1 -3 0 222.28 5.90 1 -3 0 223.08 6.00 -1 -3 0 233.48 6.00 -1 -3 0 230.68 6.10 1 -3 0 231.68 6.10 -1 -3 0 237.38 6.00 1 3 0 215.68 5.90 -1 3 0 228.08 5.90 -1 3 0 229.78 6.10 -1 3 0 235.48 6.00 1 3 0 231.88 6.00 1 3 0 232.48 6.10 3 -3 0 760.02 17.50 -3 -3 0 762.62 17.50 -3 -3 0 755.72 17.50 -3 -3 0 750.22 17.60 3 -3 0 752.92 17.50 3 -3 0 734.43 17.50 3 3 0 748.63 17.50 -3 3 0 747.33 17.50 -3 3 0 746.63 17.40 3 3 0 778.32 17.50 -3 3 0 754.62 17.40 5 -3 0 20.10 1.30 -5 -3 0 19.40 1.40 5 -3 0 20.60 1.40 -5 -3 0 19.60 1.40 -5 -3 0 21.70 1.50 5 -3 0 18.90 1.30 5 3 0 19.60 1.40 -5 3 0 18.70 1.30 5 3 0 21.00 1.40 -5 3 0 20.90 1.40 -5 3 0 19.80 1.30 7 -3 0 137.59 4.00 -7 -3 0 143.09 4.20 7 -3 0 146.89 4.30 -7 -3 0 140.99 4.20 7 -3 0 137.79 4.10 -7 -3 0 142.19 4.30 -7 3 0 142.89 4.10 7 3 0 136.49 4.20 -7 3 0 145.59 4.10 7 3 0 143.49 4.30 -7 3 0 142.99 4.10 -9 -3 0 8.80 1.10 9 -3 0 8.10 1.10 -9 -3 0 8.70 1.20 9 -3 0 6.70 1.00 9 -3 0 7.30 0.90 -9 -3 0 6.90 1.00 -9 3 0 8.60 1.10 9 3 0 6.40 1.00 -9 3 0 7.10 0.90 9 3 0 7.40 1.00 -9 3 0 7.50 1.00 11 -3 0 19.10 1.70 11 -3 0 18.60 1.30 11 -3 0 17.20 1.60 -11 -3 0 20.10 1.70 -11 -3 0 17.40 1.70 -11 -3 0 18.20 1.60 11 3 0 16.20 1.60 -11 3 0 19.70 1.60 -11 3 0 18.80 1.60 11 3 0 15.50 1.70 13 -3 0 2.40 0.70 13 -3 0 0.90 1.00 -13 -3 0 1.50 1.00 -13 -3 0 1.10 0.90 13 -3 0 1.40 1.00 -13 -3 0 1.40 1.00 13 3 0 0.70 1.00 -13 3 0 1.50 0.90 -13 3 0 1.70 1.00 13 3 0 1.20 1.00 -15 -3 0 2.00 1.00 15 -3 0 1.40 0.60 15 -3 0 0.70 1.00 15 -3 0 2.10 1.10 -15 -3 0 1.30 1.10 -15 -3 0 1.40 1.10 -15 3 0 1.60 1.00 15 3 0 2.90 1.30 -15 3 0 0.80 1.00 -17 -3 0 2.10 1.20 17 -3 0 0.60 1.20 17 -3 0 -1.70 1.20 -17 -3 0 0.60 1.20 -17 -3 0 0.70 1.20 17 3 0 1.70 1.40 -17 3 0 1.50 1.10 17 3 0 -0.80 1.20 -17 3 0 1.60 1.10 19 -3 0 84.99 4.10 -19 -3 0 86.89 3.70 19 -3 0 90.89 4.10 -19 3 0 83.39 3.50 19 3 0 90.49 4.30 -19 3 0 81.89 3.60 19 3 0 88.69 4.10 21 -3 0 448.06 12.10 -21 -3 0 426.96 11.60 -21 -3 0 441.16 11.30 21 -3 0 436.86 12.00 -21 -3 0 446.16 11.70 21 3 0 439.06 12.20 -21 3 0 443.86 11.30 -21 3 0 442.26 11.30 21 3 0 442.56 12.20 -23 -3 0 41.80 3.10 -23 -3 0 46.80 3.70 23 -3 0 47.60 4.10 -23 -3 0 44.60 4.00 -23 3 0 46.70 3.40 -23 3 0 44.80 3.30 23 3 0 41.30 4.20 23 3 0 54.59 4.50 25 -3 0 5.90 2.70 -25 -3 0 -1.70 1.70 -25 -3 0 4.20 2.30 -25 -3 0 2.90 2.40 25 -3 0 8.20 2.90 25 3 0 8.20 3.60 -25 3 0 0.90 1.90 25 3 0 2.90 2.70 -25 3 0 4.30 2.10 0 -4 0 763.42 18.30 0 -4 0 808.12 18.30 0 -4 0 790.32 18.50 0 4 0 762.32 18.20 0 4 0 752.32 18.20 -2 -4 0 676.53 15.40 -2 -4 0 641.54 15.40 2 -4 0 635.54 15.40 2 -4 0 624.94 15.40 -2 -4 0 618.24 15.50 2 -4 0 646.64 15.40 -2 4 0 670.53 15.40 2 4 0 659.33 15.40 2 4 0 652.63 15.40 -2 4 0 600.04 15.20 -2 4 0 636.44 15.40 -4 -4 0 101.49 3.70 -4 -4 0 101.59 3.60 4 -4 0 106.19 3.60 -4 -4 0 104.19 3.60 4 -4 0 110.09 3.60 4 -4 0 106.59 3.70 -4 4 0 103.99 3.60 -4 4 0 105.99 3.60 4 4 0 107.39 3.70 4 4 0 105.49 3.70 -4 4 0 109.09 3.60 6 -4 0 319.67 8.10 6 -4 0 298.97 8.10 -6 -4 0 303.27 8.30 6 -4 0 295.17 8.00 -6 -4 0 311.57 8.10 -6 -4 0 305.27 8.10 6 4 0 309.77 8.20 -6 4 0 308.97 8.00 -6 4 0 319.37 8.10 6 4 0 299.87 8.10 -6 4 0 306.47 8.00 -8 -4 0 115.09 4.10 -8 -4 0 114.39 4.00 8 -4 0 122.89 4.00 -8 -4 0 115.29 3.90 8 -4 0 115.89 4.00 8 -4 0 113.19 3.80 8 4 0 114.49 4.00 8 4 0 111.79 4.00 -8 4 0 116.29 3.90 -8 4 0 118.09 3.90 10 -4 0 163.18 5.10 10 -4 0 159.48 5.00 -10 -4 0 155.28 5.10 -10 -4 0 163.18 5.10 -10 -4 0 155.08 5.00 10 -4 0 152.18 4.70 10 4 0 154.78 5.00 10 4 0 155.28 5.10 -10 4 0 154.78 4.80 -10 4 0 160.98 4.90 12 -4 0 97.89 3.40 12 -4 0 100.89 3.80 -12 -4 0 96.49 3.80 -12 -4 0 96.39 3.80 -12 -4 0 94.49 3.90 12 -4 0 97.89 3.90 12 4 0 96.79 3.90 12 4 0 94.19 4.00 -12 4 0 99.69 3.70 -12 4 0 96.69 3.60 -14 -4 0 50.49 2.90 14 -4 0 42.70 2.80 14 -4 0 46.80 2.80 14 -4 0 47.70 2.40 -14 -4 0 39.00 3.00 -14 -4 0 49.20 2.90 -14 4 0 48.50 2.70 -14 4 0 44.80 2.70 14 4 0 44.70 3.10 14 4 0 48.00 2.90 16 -4 0 85.49 3.00 16 -4 0 82.09 3.90 -16 -4 0 81.29 3.80 -16 -4 0 81.39 3.80 16 -4 0 85.49 3.90 -16 -4 0 86.29 3.90 16 4 0 88.69 4.00 16 4 0 77.89 4.00 -16 4 0 85.29 3.70 -16 4 0 81.19 3.60 18 -4 0 9.50 1.90 18 -4 0 12.10 1.50 -18 -4 0 8.50 1.80 -18 -4 0 7.20 2.40 18 -4 0 11.60 1.90 -18 4 0 11.00 1.80 18 4 0 10.50 2.10 18 4 0 10.30 2.10 -18 4 0 8.60 1.70 -20 -4 0 0.10 1.70 20 -4 0 1.30 1.90 -20 -4 0 1.60 1.80 -20 -4 0 0.10 1.80 20 -4 0 1.60 1.90 -20 4 0 2.50 1.70 20 4 0 1.70 2.10 20 4 0 -0.40 2.70 -20 4 0 -1.30 1.70 -22 -4 0 4.80 2.30 22 -4 0 7.80 2.20 22 -4 0 5.40 2.30 -22 -4 0 4.80 2.20 -22 4 0 9.00 2.10 22 4 0 6.70 2.50 22 4 0 4.80 2.60 -24 -4 0 23.20 3.00 -24 -4 0 28.10 3.40 -24 -4 0 21.10 2.90 24 -4 0 29.30 3.50 24 4 0 33.10 3.90 1 -5 0 29.60 2.20 -1 -5 0 28.80 2.20 -1 -5 0 28.20 2.20 -1 -5 0 27.90 2.10 1 -5 0 33.20 2.20 1 -5 0 28.40 2.10 1 5 0 28.20 2.10 -1 5 0 30.60 2.10 -1 5 0 31.30 2.30 1 5 0 32.70 2.20 -3 -5 0 14.90 1.90 3 -5 0 12.40 1.50 3 -5 0 13.80 1.70 3 -5 0 11.10 1.50 -3 -5 0 12.60 1.60 -3 -5 0 12.70 1.50 3 5 0 12.40 1.60 -3 5 0 11.90 1.50 3 5 0 9.90 1.50 -3 5 0 11.20 1.40 -5 -5 0 814.02 19.00 5 -5 0 766.02 18.90 -5 -5 0 782.92 19.00 -5 -5 0 773.12 19.70 5 -5 0 791.52 18.90 5 -5 0 759.22 19.10 -5 5 0 763.42 18.70 5 5 0 807.92 19.00 -5 5 0 804.72 18.90 -7 -5 0 47.10 3.20 7 -5 0 45.70 2.60 7 -5 0 38.30 3.00 7 -5 0 44.10 2.60 -7 -5 0 46.40 2.60 7 5 0 43.10 2.70 -7 5 0 44.80 2.70 -7 5 0 44.80 2.70 7 5 0 41.50 2.70 -9 -5 0 17.10 2.00 9 -5 0 14.90 1.70 9 -5 0 15.70 2.00 -9 -5 0 17.20 1.90 9 -5 0 16.60 2.10 -9 -5 0 15.90 1.90 -9 5 0 12.80 1.70 9 5 0 16.60 2.00 -9 5 0 19.50 2.20 11 -5 0 41.10 2.70 -11 -5 0 31.40 3.40 11 -5 0 41.40 2.80 -11 -5 0 43.10 3.00 -11 -5 0 43.00 2.80 11 -5 0 45.80 2.90 -11 5 0 40.70 2.80 -11 5 0 39.80 2.80 11 5 0 43.80 2.90 11 5 0 45.00 2.60 -13 -5 0 47.50 3.10 -13 -5 0 49.80 3.40 -13 -5 0 46.80 3.10 13 -5 0 44.10 3.10 13 -5 0 46.70 3.00 13 -5 0 45.10 2.90 -13 5 0 47.30 3.00 13 5 0 46.20 3.10 13 5 0 44.80 3.10 -15 -5 0 2.70 1.70 15 -5 0 2.00 1.50 15 -5 0 4.90 1.50 -15 -5 0 2.60 1.60 15 -5 0 3.10 1.70 -15 -5 0 2.30 1.60 15 5 0 1.60 1.60 -15 5 0 3.30 1.60 15 5 0 -0.80 1.60 -15 5 0 2.40 1.60 -17 -5 0 10.50 2.10 17 -5 0 6.30 2.00 -17 -5 0 9.70 2.10 -17 -5 0 8.40 2.10 17 -5 0 8.70 1.60 17 -5 0 5.50 1.90 -17 5 0 5.60 1.90 -17 5 0 8.30 1.90 17 5 0 4.00 2.10 -19 -5 0 5.10 2.30 19 -5 0 6.40 2.30 -19 -5 0 6.60 2.40 19 -5 0 7.00 1.50 19 -5 0 5.90 2.30 -19 -5 0 8.40 2.40 19 5 0 8.90 2.50 -19 5 0 3.30 2.00 19 5 0 7.40 2.70 -21 -5 0 11.40 2.80 -21 -5 0 10.90 2.90 21 -5 0 12.60 2.90 -21 -5 0 14.80 2.90 21 -5 0 12.10 2.70 -21 5 0 12.10 2.60 21 5 0 15.50 3.40 0 -6 0 384.76 10.40 0 -6 0 379.06 10.50 0 -6 0 387.26 10.70 0 6 0 373.66 10.30 0 6 0 389.26 10.50 -2 -6 0 24.20 2.20 2 -6 0 20.70 2.30 -2 -6 0 25.80 2.30 2 -6 0 21.60 2.20 2 -6 0 24.70 2.40 -2 -6 0 21.30 2.30 -2 6 0 20.80 2.50 2 6 0 20.80 2.40 -2 6 0 24.00 2.50 2 6 0 23.10 2.50 -4 -6 0 29.00 2.40 4 -6 0 26.30 2.50 -4 -6 0 26.60 2.70 4 -6 0 30.90 2.40 4 -6 0 29.60 2.40 -4 -6 0 31.80 2.60 -4 6 0 33.70 3.10 4 6 0 33.60 2.60 4 6 0 31.40 2.50 -4 6 0 24.70 2.60 -6 -6 0 76.19 3.70 -6 -6 0 70.59 3.50 6 -6 0 70.99 3.40 -6 -6 0 64.69 3.70 6 -6 0 74.59 3.50 6 -6 0 68.09 3.70 6 6 0 64.59 3.60 -6 6 0 70.29 3.70 -6 6 0 73.89 3.70 6 6 0 71.39 3.50 -8 -6 0 315.17 9.10 -8 -6 0 310.57 9.00 -8 -6 0 304.87 9.30 8 -6 0 309.97 9.00 8 -6 0 297.67 8.90 8 -6 0 307.77 9.00 -8 6 0 297.47 8.80 -8 6 0 319.57 8.90 8 6 0 306.77 9.10 8 6 0 312.37 9.00 -10 -6 0 13.40 2.00 10 -6 0 9.80 1.90 10 -6 0 10.90 1.80 -10 -6 0 11.20 1.90 -10 -6 0 9.80 2.00 10 -6 0 11.50 1.90 -10 6 0 10.00 1.80 10 6 0 10.60 1.80 -10 6 0 11.90 2.00 10 6 0 9.20 1.80 -12 -6 0 44.50 3.80 -12 -6 0 43.90 3.40 12 -6 0 50.89 3.60 12 -6 0 42.50 3.60 -12 -6 0 43.20 3.50 12 -6 0 42.50 3.50 -12 6 0 46.00 3.50 -12 6 0 41.30 3.50 12 6 0 58.29 3.70 12 6 0 46.50 3.80 14 -6 0 75.59 4.30 -14 -6 0 77.89 4.40 -14 -6 0 71.19 4.50 14 -6 0 73.59 5.20 -14 -6 0 68.99 4.50 14 -6 0 76.99 4.50 14 6 0 73.49 4.50 14 6 0 71.29 4.10 -14 6 0 61.59 4.10 -14 6 0 72.29 4.20 16 -6 0 49.40 4.10 -16 -6 0 39.30 4.00 16 -6 0 36.90 4.50 16 -6 0 31.70 4.10 -16 -6 0 39.60 4.90 16 6 0 32.80 3.90 16 6 0 42.10 4.00 -16 6 0 35.00 3.90 -16 6 0 48.40 4.10 18 -6 0 15.00 2.40 -18 -6 0 18.20 3.30 18 -6 0 18.60 3.20 18 -6 0 19.20 3.00 -18 -6 0 17.80 3.00 -18 -6 0 14.00 3.20 -18 6 0 14.60 2.90 -18 6 0 16.10 2.70 18 6 0 18.50 3.40 1 -7 0 -0.90 1.40 -1 -7 0 -1.10 1.40 1 -7 0 2.60 1.60 1 -7 0 1.40 1.60 -1 -7 0 -1.30 1.40 -1 -7 0 1.70 1.50 1 7 0 1.00 1.70 -1 7 0 1.10 1.80 -1 7 0 0.00 1.90 1 7 0 -3.50 1.60 -3 -7 0 -0.70 1.40 3 -7 0 4.30 1.70 3 -7 0 -0.80 1.70 -3 -7 0 1.90 1.60 3 -7 0 2.10 1.40 -3 -7 0 0.40 1.50 -3 7 0 0.00 1.80 3 7 0 0.70 1.70 3 7 0 1.30 1.80 -3 7 0 -0.10 1.80 -5 -7 0 208.38 7.00 5 -7 0 201.18 6.80 -5 -7 0 199.98 7.90 5 -7 0 185.58 7.10 5 7 0 203.68 7.10 -5 7 0 204.28 7.10 -5 7 0 201.68 6.90 -7 -7 0 30.30 3.40 7 -7 0 28.50 3.40 7 -7 0 36.10 3.20 7 -7 0 33.00 3.30 -7 -7 0 35.70 3.60 7 7 0 34.40 3.50 -7 7 0 33.70 3.80 7 7 0 29.90 3.40 -7 7 0 28.60 3.60 -9 -7 0 3.60 2.10 9 -7 0 5.70 1.90 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269.57 6.30 -5 -1 1 271.77 6.40 -5 -1 1 275.27 6.30 5 -1 -1 267.07 6.30 5 1 -1 264.57 6.40 -5 1 1 267.77 6.20 -5 1 1 279.77 6.30 5 1 -1 259.67 6.40 5 1 -1 272.77 6.40 3 -1 -1 0.30 0.30 -3 -1 1 0.20 0.30 3 -1 -1 -0.30 0.30 -3 -1 1 0.40 0.30 -3 -1 1 0.00 0.30 3 1 -1 -0.30 0.30 3 1 -1 0.60 0.40 -3 1 1 -0.10 0.30 3 1 -1 0.40 0.30 -3 1 1 0.20 0.30 -1 -1 1 43.00 1.40 1 -1 -1 40.60 1.30 -1 -1 1 43.20 1.30 1 -1 -1 42.20 1.30 -1 -1 1 40.80 1.30 -1 1 1 38.80 1.20 -1 1 1 42.80 1.30 1 1 -1 43.60 1.40 1 1 -1 43.40 1.30 1 1 -1 43.80 1.30 1 -1 1 399.66 9.30 1 -1 1 416.46 9.40 1 -1 1 397.46 9.30 -1 -1 -1 398.66 9.30 -1 -1 -1 393.06 9.30 -1 1 -1 414.96 9.30 -1 1 -1 419.76 9.30 1 1 1 405.36 9.30 1 1 1 415.46 9.30 -1 1 -1 408.66 9.40 3 -1 1 7.70 0.70 3 -1 1 7.90 0.70 -3 -1 -1 6.80 0.70 3 -1 1 7.30 0.60 -3 -1 -1 8.30 0.80 -3 1 -1 6.20 0.70 -3 1 -1 6.70 0.70 -3 1 -1 8.80 0.70 3 1 1 8.10 0.80 3 1 1 7.00 0.70 5 -1 1 25.30 1.00 5 -1 1 25.50 1.20 -5 -1 -1 24.10 1.20 5 -1 1 26.50 1.20 -5 -1 -1 27.60 1.30 -5 1 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139.19 5.00 -2 -4 9 147.09 4.40 2 -4 -9 138.69 5.10 -2 -4 9 139.29 5.60 -2 -4 9 145.79 4.40 2 4 -9 141.29 5.20 2 4 -9 145.59 5.50 2 4 -9 131.49 5.70 0 -4 9 4.60 1.30 0 -4 -9 1.60 1.40 0 -4 9 3.40 1.20 0 -4 -9 1.80 1.50 0 -4 9 1.60 1.50 0 4 -9 3.20 1.60 0 4 9 0.60 0.70 0 4 9 1.50 0.80 0 4 -9 1.80 1.60 0 4 -9 3.50 1.60 2 -4 9 5.50 1.60 -2 -4 -9 5.00 1.60 -2 -4 -9 0.60 1.80 2 -4 9 5.10 1.40 2 -4 9 4.20 1.40 -2 4 -9 2.30 1.70 2 4 9 1.50 1.00 -2 4 -9 5.30 1.70 -2 4 -9 1.60 1.60 2 4 9 2.90 1.10 4 -4 9 167.18 7.10 4 -4 9 196.28 6.00 -4 -4 -9 187.78 6.40 4 -4 9 193.08 6.80 -4 -4 -9 192.28 6.40 -4 4 -9 190.28 6.50 4 4 9 187.58 5.60 4 4 9 194.58 5.70 -4 4 -9 186.98 6.40 -4 4 -9 188.38 6.70 6 -4 9 181.98 6.20 -6 -4 -9 181.88 6.40 6 -4 9 191.58 6.20 6 -4 9 189.78 7.00 -6 -4 -9 186.68 6.50 6 4 9 176.08 5.80 -6 4 -9 181.68 6.50 6 4 9 186.18 5.90 -6 4 -9 186.08 6.60 -6 4 -9 191.98 6.90 -8 -4 -9 5.10 2.00 8 -4 9 1.40 1.80 -8 -4 -9 0.60 1.90 8 -4 9 1.10 1.60 8 -4 9 4.80 1.80 -8 4 -9 2.60 2.10 8 4 9 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-12 86.69 4.90 13 3 -12 104.39 6.60 13 3 -12 84.89 5.30 11 -3 -12 13.10 1.90 11 -3 -12 15.20 1.90 11 -3 -12 13.50 3.30 11 3 -12 15.70 3.30 11 3 -12 13.50 2.40 11 3 -12 15.60 2.50 9 -3 -12 -3.50 2.60 9 -3 -12 1.80 1.60 9 -3 -12 -2.10 1.70 9 3 -12 6.40 3.00 9 3 -12 -1.10 1.90 9 3 -12 0.10 2.30 7 -3 -12 -4.80 2.30 7 -3 -12 1.90 1.60 7 -3 -12 -2.30 1.60 7 3 -12 3.50 2.50 7 3 -12 3.50 2.00 5 -3 -12 -1.20 1.70 5 -3 -12 2.30 1.70 5 3 -12 -1.70 2.00 5 3 -12 0.60 2.30 5 3 -12 -2.30 1.80 3 -3 -12 2.90 1.80 3 -3 -12 0.50 2.10 3 3 -12 2.10 2.00 3 3 -12 4.80 2.20 3 3 -12 1.80 2.00 1 -3 -12 52.99 3.80 1 -3 -12 54.49 4.50 1 3 -12 55.79 3.90 1 3 -12 49.30 3.90 1 3 -12 51.79 4.00 -1 -3 -12 21.70 2.60 -1 -3 -12 15.40 2.50 -1 3 -12 25.20 3.30 -1 3 -12 16.80 2.80 -1 3 -12 17.50 2.60 -3 -3 -12 1.10 2.10 -3 -3 -12 2.40 2.20 3 -3 12 1.10 1.30 3 -3 12 0.20 1.20 -3 3 -12 2.70 2.40 -3 3 -12 1.40 2.00 -3 3 -12 -1.00 2.20 -5 -3 -12 22.40 3.00 -5 -3 -12 32.80 4.20 5 -3 12 27.30 2.90 5 -3 12 23.90 2.90 -5 3 -12 24.00 3.10 -5 3 -12 29.10 3.50 -5 3 -12 28.90 3.20 -7 -3 -12 0.70 2.50 -7 -3 -12 -2.70 2.50 7 -3 12 -1.80 1.90 7 3 12 -0.50 1.60 -7 3 -12 -0.20 2.70 -7 3 -12 4.00 2.50 7 3 12 0.20 1.50 -7 3 -12 -3.70 2.50 9 -3 12 44.50 4.00 -9 -3 -12 37.50 4.70 9 -3 12 36.00 4.00 -9 -3 -12 43.70 5.00 9 3 12 35.00 3.70 -9 3 -12 41.10 4.80 9 3 12 41.50 4.40 -9 3 -12 46.80 5.00 -9 3 -12 47.80 5.10 11 -3 12 8.30 2.50 -11 -3 -12 7.40 3.30 11 -3 12 1.50 3.00 11 3 12 6.30 2.50 11 3 12 3.60 2.70 -11 3 -12 8.90 3.50 -11 3 -12 8.90 3.20 10 4 -12 -2.80 2.70 10 4 -12 0.40 3.50 8 -4 -12 6.90 2.30 8 -4 -12 4.20 2.20 8 4 -12 9.20 3.20 8 4 -12 2.20 2.50 8 4 -12 3.90 2.70 6 -4 -12 3.30 2.10 6 4 -12 5.90 3.00 6 4 -12 1.10 2.60 6 4 -12 6.40 2.50 4 -4 -12 27.70 2.90 4 -4 -12 22.00 2.70 4 4 -12 30.10 3.40 4 4 -12 24.20 3.40 4 4 -12 28.40 3.30 2 -4 -12 31.50 4.00 2 -4 -12 32.80 4.00 2 4 -12 26.70 3.40 2 4 -12 46.70 4.50 2 4 -12 34.20 3.90 0 -4 -12 6.60 2.50 0 -4 -12 7.80 2.50 0 4 -12 -1.70 2.40 0 4 -12 6.20 2.90 0 4 -12 8.20 2.60 2 -4 12 0.70 1.60 -2 -4 -12 5.60 2.80 -2 -4 -12 3.30 2.60 2 -4 12 1.00 1.50 -2 4 -12 1.10 2.60 -2 4 -12 1.70 2.70 -2 4 -12 -2.10 2.50 4 -4 12 0.60 1.80 -4 -4 -12 1.80 2.60 -4 -4 -12 3.90 2.60 -4 4 -12 -2.50 2.90 -4 4 -12 2.50 2.50 -4 4 -12 -5.00 2.60 4 4 12 -1.30 1.00 4 4 12 -0.20 0.90 -6 -4 -12 10.00 3.10 6 -4 12 12.90 2.50 -6 -4 -12 19.70 3.30 6 -4 12 11.80 2.60 -6 4 -12 10.80 3.30 -6 4 -12 18.50 4.00 -6 4 -12 17.60 3.50 -8 -4 -12 8.50 3.50 8 -4 12 5.60 2.70 8 -4 12 5.80 2.50 8 4 12 1.70 2.10 8 4 12 2.70 2.40 -8 4 -12 11.30 3.60 -8 4 -12 1.40 3.30 12 0 -13 1.50 2.90 12 0 -13 -0.70 2.00 10 0 -13 -1.80 2.70 10 0 -13 0.40 1.20 10 0 -13 -0.80 1.20 8 0 -13 -1.10 1.30 8 0 -13 0.90 2.60 8 0 -13 -1.60 1.30 6 0 -13 -0.80 1.40 6 0 -13 -2.30 2.50 6 0 -13 -1.30 1.40 4 0 -13 -0.30 2.40 4 0 -13 1.30 1.60 4 0 -13 0.20 1.60 2 0 -13 -0.70 2.10 2 0 -13 0.10 1.60 0 0 -13 1.60 1.90 0 0 -13 3.80 2.10 -2 0 -13 2.20 2.00 -2 0 -13 -0.20 1.90 -2 0 -13 0.10 2.00 -4 0 -13 1.60 2.10 -4 0 -13 0.10 2.00 -4 0 -13 5.50 2.20 -6 0 -13 2.90 2.20 6 0 13 1.30 1.10 -6 0 -13 2.10 2.40 6 0 13 0.50 1.20 -6 0 -13 -1.50 2.60 8 0 13 0.40 1.60 -8 0 -13 6.00 2.60 -8 0 -13 -2.40 2.40 -8 0 -13 0.30 2.60 8 0 13 -0.40 1.70 10 0 13 -0.30 2.20 -10 0 -13 0.80 3.00 -10 0 -13 4.30 3.10 -10 0 -13 4.10 2.70 -12 0 -13 2.80 3.20 12 0 13 -3.00 2.60 12 0 13 -1.30 2.40 13 -1 -13 47.60 5.70 13 1 -13 45.50 5.50 11 -1 -13 28.00 3.80 11 -1 -13 22.00 2.90 11 1 -13 24.20 2.10 11 1 -13 24.40 3.60 11 1 -13 26.60 2.50 9 -1 -13 2.70 2.80 9 -1 -13 -2.90 1.20 9 1 -13 -0.80 2.70 9 1 -13 0.70 1.60 9 1 -13 -0.40 1.60 7 -1 -13 13.10 2.90 7 -1 -13 7.70 1.60 7 1 -13 10.70 1.80 7 1 -13 12.80 3.10 7 1 -13 9.80 1.90 5 -1 -13 6.40 2.60 5 -1 -13 5.40 1.70 5 -1 -13 7.10 1.70 5 1 -13 6.10 1.90 5 1 -13 5.50 2.50 5 1 -13 9.60 1.90 3 -1 -13 1.30 2.20 3 -1 -13 1.80 1.70 3 -1 -13 2.30 1.80 3 1 -13 0.70 2.30 3 1 -13 0.40 2.20 3 1 -13 3.80 1.80 1 -1 -13 8.10 2.10 1 -1 -13 8.10 2.10 1 -1 -13 10.40 2.60 1 1 -13 4.70 3.10 1 1 -13 11.20 2.10 1 1 -13 10.50 2.40 -1 -1 -13 25.80 2.70 -1 -1 -13 23.30 2.80 -1 -1 -13 28.50 3.50 -1 1 -13 28.00 2.90 -1 1 -13 22.10 2.60 -1 1 -13 27.20 2.80 -3 -1 -13 16.40 2.30 -3 -1 -13 22.10 2.80 -3 1 -13 15.40 2.70 -3 1 -13 17.10 2.70 -3 1 -13 15.40 2.60 -5 -1 -13 26.40 3.00 -5 -1 -13 24.20 2.80 -5 1 -13 19.90 2.60 -5 1 -13 21.40 3.20 -5 1 -13 22.90 3.10 -7 -1 -13 81.89 5.00 -7 -1 -13 73.89 5.20 7 -1 13 79.79 3.70 -7 1 -13 71.19 4.90 7 1 13 60.19 3.20 -7 1 -13 71.49 5.20 -7 1 -13 65.69 4.90 9 -1 13 32.20 3.50 -9 -1 -13 25.00 3.50 9 -1 13 34.00 3.70 -9 -1 -13 40.90 4.50 -9 -1 -13 27.90 3.40 -9 1 -13 34.70 4.50 9 1 13 30.50 3.30 -9 1 -13 30.60 3.50 -9 1 -13 22.70 3.40 11 -1 13 2.20 2.50 -11 -1 -13 3.50 3.20 11 -1 13 2.20 2.40 -11 -1 -13 2.40 3.10 11 1 13 5.20 2.30 -11 1 -13 1.20 2.90 11 1 13 0.60 2.60 -11 1 -13 -1.30 3.20 10 -2 -13 18.50 2.40 10 -2 -13 12.40 1.80 10 -2 -13 10.70 3.40 10 2 -13 15.50 3.40 10 2 -13 13.00 2.30 10 2 -13 14.90 2.40 8 -2 -13 26.50 2.80 8 -2 -13 20.80 3.20 8 -2 -13 22.00 2.80 8 2 -13 30.80 3.80 8 2 -13 22.50 2.50 8 2 -13 23.00 3.60 6 -2 -13 12.90 2.00 6 -2 -13 14.00 3.20 6 -2 -13 11.70 1.90 6 2 -13 13.60 2.20 6 2 -13 11.00 2.90 6 2 -13 11.40 2.30 4 -2 -13 68.29 3.90 4 -2 -13 80.19 4.10 4 -2 -13 72.99 5.20 4 2 -13 75.79 4.30 4 2 -13 77.89 5.20 2 -2 -13 25.70 3.30 2 -2 -13 35.80 3.70 2 -2 -13 32.70 4.30 2 2 -13 37.50 3.80 2 2 -13 36.30 4.20 2 2 -13 37.50 3.80 0 -2 -13 2.90 2.20 0 -2 -13 -3.70 2.20 0 -2 -13 -1.50 2.00 0 2 -13 2.50 2.20 0 2 -13 -1.40 2.10 0 2 -13 3.20 2.30 -2 -2 -13 29.00 3.00 -2 -2 -13 29.00 3.00 -2 -2 -13 31.60 4.10 -2 2 -13 26.90 3.00 -2 2 -13 29.60 3.20 -2 2 -13 30.70 3.90 -4 -2 -13 176.78 7.20 -4 -2 -13 175.98 7.00 -4 -2 -13 185.18 7.00 -4 2 -13 176.78 7.00 -4 2 -13 179.28 7.10 -6 -2 -13 19.10 3.10 -6 -2 -13 22.80 3.40 -6 -2 -13 19.50 2.90 6 -2 13 23.10 2.90 -6 2 -13 22.70 3.10 -6 2 -13 24.30 3.50 -6 2 -13 21.80 3.30 -8 -2 -13 -3.90 2.60 -8 -2 -13 2.60 2.90 8 -2 13 2.50 2.00 -8 -2 -13 -2.10 2.90 8 -2 13 6.90 2.30 8 2 13 1.20 1.60 -8 2 -13 0.10 2.80 -8 2 -13 -0.80 3.00 -8 2 -13 4.40 2.90 8 2 13 1.90 1.80 10 -2 13 43.20 4.20 -10 -2 -13 34.10 4.20 -10 -2 -13 29.70 4.70 10 -2 13 40.40 4.40 10 2 13 33.30 3.20 -10 2 -13 30.10 4.10 -10 2 -13 40.70 4.30 9 -3 -13 -0.70 2.00 9 -3 -13 -5.00 3.20 9 3 -13 3.30 2.60 9 3 -13 10.20 3.60 9 3 -13 -1.40 2.50 7 -3 -13 3.40 2.10 7 -3 -13 5.00 2.10 7 -3 -13 3.30 3.00 7 3 -13 1.40 2.50 7 3 -13 3.70 3.20 7 3 -13 2.60 2.50 5 -3 -13 6.20 2.20 5 -3 -13 0.30 3.10 5 -3 -13 7.60 2.10 5 3 -13 3.80 2.50 5 3 -13 9.90 3.20 5 3 -13 -0.90 2.30 3 -3 -13 3.10 2.30 3 -3 -13 0.30 2.20 3 3 -13 0.20 2.30 3 3 -13 3.60 2.80 3 3 -13 -1.40 2.40 1 -3 -13 50.39 4.30 1 -3 -13 50.19 4.30 1 3 -13 44.70 4.20 1 3 -13 39.80 4.80 1 3 -13 41.30 4.50 -1 -3 -13 10.80 2.70 -1 -3 -13 8.00 2.60 -1 3 -13 13.10 2.50 -1 3 -13 9.00 4.80 -1 3 -13 8.10 2.90 3 -3 13 1.60 1.20 -3 -3 -13 0.50 2.60 3 -3 13 1.00 1.10 -3 3 -13 -3.50 2.70 -3 3 -13 0.90 2.60 -3 3 -13 -4.00 2.80 -5 -3 -13 37.50 3.90 5 -3 13 29.20 3.10 -5 -3 -13 44.30 4.20 -5 3 -13 22.10 3.10 -5 3 -13 34.40 4.00 -5 3 -13 29.60 3.90 -7 -3 -13 5.20 3.30 7 -3 13 2.30 2.10 -7 -3 -13 5.70 3.10 7 -3 13 0.90 3.40 -7 3 -13 -1.70 2.90 7 3 13 -1.10 2.30 -7 3 -13 5.40 3.30 0 -4 -13 5.20 2.90 0 4 -13 -6.60 3.10 0 4 -13 1.80 3.30 8 0 -14 7.90 3.30 8 0 -14 7.60 1.90 8 0 -14 11.10 3.40 6 0 -14 9.40 3.10 6 0 -14 10.90 2.10 6 0 -14 13.20 2.20 4 0 -14 180.78 8.00 4 0 -14 191.48 6.50 4 0 -14 194.98 6.40 2 0 -14 1096.79 26.20 2 0 -14 1108.89 26.30 2 0 -14 1114.09 28.00 0 0 -14 83.89 4.90 0 0 -14 87.49 4.90 0 0 -14 97.79 5.80 -2 0 -14 285.77 9.00 -2 0 -14 272.57 9.60 -2 0 -14 278.67 9.00 -4 0 -14 60.29 4.90 -4 0 -14 44.20 4.90 -4 0 -14 55.29 4.70 -6 0 -14 44.80 4.60 -6 0 -14 58.09 5.30 -6 0 -14 53.89 5.50 7 -1 -14 0.90 3.20 7 -1 -14 -3.30 1.80 7 1 -14 -6.70 3.10 7 1 -14 0.90 2.10 7 1 -14 -3.40 2.20 5 -1 -14 69.69 5.70 5 -1 -14 49.00 4.20 5 1 -14 55.49 4.00 5 1 -14 55.19 4.80 5 1 -14 55.79 5.70 3 -1 -14 15.70 2.50 3 -1 -14 17.50 3.50 3 1 -14 16.00 3.40 3 1 -14 20.00 2.80 3 1 -14 18.20 2.60 1 -1 -14 21.90 2.80 1 -1 -14 25.70 3.60 1 1 -14 27.40 3.10 1 1 -14 25.30 2.90 1 1 -14 29.30 3.90 -1 -1 -14 65.79 4.90 -1 -1 -14 62.59 4.70 -1 1 -14 58.29 5.00 -1 1 -14 69.29 4.80 -1 1 -14 62.29 4.90 -3 -1 -14 149.79 7.20 -3 -1 -14 135.19 6.60 -3 1 -14 137.39 6.50 -3 1 -14 137.49 6.70 -5 -1 -14 0.80 3.00 -5 -1 -14 2.30 2.60 -5 -1 -14 7.00 3.00 -5 1 -14 3.00 3.00 -5 1 -14 -2.90 2.80 -5 1 -14 -3.90 2.90 -7 -1 -14 105.69 6.60 -7 -1 -14 117.09 6.40 -7 1 -14 108.79 6.70 -7 1 -14 97.19 6.50 6 -2 -14 20.80 2.70 6 -2 -14 17.20 3.90 6 -2 -14 16.80 3.80 6 2 -14 17.20 3.10 6 2 -14 19.70 3.80 6 2 -14 19.60 2.90 4 -2 -14 51.89 4.10 4 -2 -14 66.69 6.00 4 2 -14 55.89 4.70 4 2 -14 47.80 5.30 4 2 -14 60.79 4.70 2 -2 -14 401.06 12.80 2 -2 -14 421.96 11.50 2 -2 -14 414.46 11.50 2 2 -14 407.26 11.70 2 2 -14 391.26 12.90 2 2 -14 435.46 11.90 0 -2 -14 199.88 8.40 0 -2 -14 201.18 7.50 0 -2 -14 223.98 7.60 0 2 -14 198.18 8.50 0 2 -14 219.18 8.00 0 2 -14 207.68 8.10 -2 -2 -14 122.39 7.70 -2 -2 -14 127.39 6.30 -2 -2 -14 107.69 6.70 -2 2 -14 133.99 6.60 -2 2 -14 124.89 7.40 -2 2 -14 112.69 6.30 -4 -2 -14 47.50 5.60 -4 -2 -14 50.39 5.30 -4 2 -14 61.09 5.70 -4 2 -14 44.40 5.60 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 20106 _shelx_res_file ; TITL mo_1501lp98_0m_a.res in C2/c mo_1501lp98_0m_a.res created by SHELXL-2018/3 at 15:04:21 on 18-Mar-2019 REM Old TITL mo_1501lp98_0m in C2/c REM SHELXT solution in C2/c REM R1 0.097, Rweak 0.002, Alpha 0.012, Orientation as input REM Formula found by SHELXT: C6 O6 CELL 0.71073 21.1667 6.6243 11.3247 90 91.509 90 ZERR 4 0.0008 0.0003 0.0004 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O UNIT 40 80 8 48 EQIV $1 +X,-Y,0.5+Z EQIV $2 1.5-X,0.5+Y,0.5-Z EQIV $3 1-X,+Y,0.5-Z L.S. 10 PLAN 10 SIZE 0.17 0.3 0.47 TEMP -173.15 HTAB O2 O3_$1 HTAB O5 O4 HTAB N O4 HTAB N O1_$2 HTAB N O6_$3 BOND $H LIST 6 MORE -1 CONF fmap 2 acta OMIT 2 0 2 OMIT 2 0 4 OMIT -2 0 6 OMIT 7 1 0 OMIT -6 0 2 REM REM REM WGHT 0.038300 1.189100 FVAR 0.38828 C1 1 0.752273 -0.013861 0.487672 11.00000 0.01146 0.01073 = 0.00906 0.00063 0.00076 -0.00121 O1 4 0.805297 -0.078882 0.505538 11.00000 0.01101 0.01905 = 0.01111 0.00006 -0.00073 0.00224 C2 1 0.723007 -0.003203 0.360237 11.00000 0.01110 0.01090 = 0.00924 0.00092 -0.00015 -0.00001 O2 4 0.714153 0.052159 0.568240 11.00000 0.01349 0.02121 = 0.00760 -0.00104 0.00035 0.00334 AFIX 147 H2 2 0.731311 0.037617 0.635430 11.00000 -1.50000 AFIX 0 O3 4 0.760727 -0.033336 0.279999 11.00000 0.01118 0.02509 = 0.00896 -0.00040 0.00141 0.00257 O4 4 0.665060 0.034931 0.347901 11.00000 0.00938 0.02185 = 0.01129 0.00373 0.00071 0.00258 N 3 0.610627 0.323417 0.189052 11.00000 0.01093 0.01427 = 0.01141 0.00143 -0.00083 -0.00094 AFIX 137 HA 2 0.626827 0.230748 0.240865 11.00000 -1.50000 HB 2 0.639850 0.352637 0.134066 11.00000 -1.50000 HC 2 0.575304 0.272353 0.152545 11.00000 -1.50000 AFIX 0 C4 1 0.594047 0.511422 0.254199 11.00000 0.01314 0.01618 = 0.01454 -0.00086 0.00124 0.00053 AFIX 23 H4A 2 0.630646 0.555335 0.304026 11.00000 -1.20000 H4B 2 0.558307 0.484025 0.306532 11.00000 -1.20000 AFIX 0 C5 1 0.575988 0.677099 0.167866 11.00000 0.01871 0.01639 = 0.02472 0.00480 0.00224 0.00101 AFIX 137 H5A 2 0.612135 0.708562 0.118768 11.00000 -1.50000 H5B 2 0.563719 0.798067 0.211491 11.00000 -1.50000 H5C 2 0.540406 0.632035 0.117391 11.00000 -1.50000 AFIX 0 C3 1 0.526814 0.030669 0.458527 11.00000 0.01024 0.01304 = 0.00996 -0.00158 0.00028 -0.00107 O5 4 0.578588 -0.068354 0.483367 11.00000 0.00948 0.02157 = 0.01574 0.00604 0.00396 0.00268 AFIX 147 H5 2 0.607761 -0.025239 0.441275 11.00000 -1.50000 AFIX 0 O6 4 0.518652 0.156376 0.381859 11.00000 0.01256 0.02017 = 0.01520 0.00643 0.00124 0.00014 HKLF 4 REM mo_1501lp98_0m_a.res in C2/c REM wR2 = 0.074678, GooF = S = 1.02880, Restrained GooF = 1.02880 for all data REM R1 = 0.028076 for 1624 Fo > 4sig(Fo) and 0.033344 for all 1829 data REM 113 parameters refined using 0 restraints END WGHT 0.0383 1.1891 REM Highest difference peak 0.495, deepest hole -0.196, 1-sigma level 0.044 Q1 1 0.7356 -0.0035 0.4245 11.00000 0.05 0.50 Q2 1 0.5000 0.0000 0.5000 10.50000 0.05 0.39 Q3 1 0.5892 0.5955 0.2096 11.00000 0.05 0.27 Q4 1 0.6026 0.4253 0.2235 11.00000 0.05 0.19 Q5 1 0.7472 -0.0732 0.2231 11.00000 0.05 0.16 Q6 1 0.7432 0.0168 0.3168 11.00000 0.05 0.15 Q7 1 0.6911 -0.0331 0.3610 11.00000 0.05 0.14 Q8 1 0.7396 -0.0485 0.3166 11.00000 0.05 0.14 Q9 1 0.6407 0.0080 0.4080 11.00000 0.05 0.14 Q10 1 0.6137 0.5305 0.2792 11.00000 0.05 0.14 ; _shelx_res_checksum 94873 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy C C1 0.75227(4) -0.01386(14) 0.48767(8) 0.01041(19) Uani d 1 O O1 0.80530(3) -0.07888(11) 0.50554(6) 0.01374(16) Uani d 1 C C2 0.72301(4) -0.00320(14) 0.36024(8) 0.01042(19) Uani d 1 O O2 0.71415(3) 0.05216(11) 0.56824(6) 0.01410(17) Uani d 1 H H2 0.731311 0.037617 0.635430 0.021 Uiso calc 1 O O3 0.76073(3) -0.03334(11) 0.28000(6) 0.01506(17) Uani d 1 O O4 0.66506(3) 0.03493(11) 0.34790(6) 0.01416(17) Uani d 1 N N 0.61063(4) 0.32342(12) 0.18905(7) 0.01222(18) Uani d 1 H HA 0.626827 0.230748 0.240865 0.018 Uiso calc 1 H HB 0.639850 0.352637 0.134066 0.018 Uiso calc 1 H HC 0.575304 0.272353 0.152545 0.018 Uiso calc 1 C C4 0.59405(5) 0.51142(15) 0.25420(9) 0.0146(2) Uani d 1 H H4A 0.630646 0.555335 0.304026 0.018 Uiso calc 1 H H4B 0.558307 0.484025 0.306532 0.018 Uiso calc 1 C C5 0.57599(5) 0.67710(16) 0.16787(10) 0.0199(2) Uani d 1 H H5A 0.612135 0.708562 0.118768 0.030 Uiso calc 1 H H5B 0.563719 0.798067 0.211491 0.030 Uiso calc 1 H H5C 0.540406 0.632035 0.117391 0.030 Uiso calc 1 C C3 0.52681(4) 0.03067(14) 0.45853(8) 0.0111(2) Uani d 1 O O5 0.57859(3) -0.06835(11) 0.48337(6) 0.01553(17) Uani d 1 H H5 0.607761 -0.025239 0.441275 0.023 Uiso calc 1 O O6 0.51865(3) 0.15638(11) 0.38186(6) 0.01596(17) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0115(4) 0.0107(4) 0.0091(4) -0.0012(3) 0.0008(3) 0.0006(3) O1 0.0110(3) 0.0190(4) 0.0111(3) 0.0022(3) -0.0007(2) 0.0001(3) C2 0.0111(4) 0.0109(4) 0.0092(4) 0.0000(3) -0.0002(3) 0.0009(3) O2 0.0135(3) 0.0212(4) 0.0076(3) 0.0033(3) 0.0003(3) -0.0010(3) O3 0.0112(3) 0.0251(4) 0.0090(3) 0.0026(3) 0.0014(2) -0.0004(3) O4 0.0094(3) 0.0218(4) 0.0113(3) 0.0026(3) 0.0007(2) 0.0037(3) N 0.0109(4) 0.0143(4) 0.0114(4) -0.0009(3) -0.0008(3) 0.0014(3) C4 0.0131(5) 0.0162(5) 0.0145(5) 0.0005(4) 0.0012(4) -0.0009(4) C5 0.0187(5) 0.0164(5) 0.0247(5) 0.0010(4) 0.0022(4) 0.0048(4) C3 0.0102(4) 0.0130(4) 0.0100(4) -0.0011(3) 0.0003(3) -0.0016(3) O5 0.0095(3) 0.0216(4) 0.0157(4) 0.0027(3) 0.0040(3) 0.0060(3) O6 0.0126(3) 0.0202(4) 0.0152(4) 0.0001(3) 0.0012(3) 0.0064(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle O1 C1 C2 . 120.93(8) O1 C1 O2 . 125.90(9) O2 C1 C2 . 113.17(8) O3 C2 C1 . 115.04(8) O3 C2 O4 . 126.56(9) O4 C2 C1 . 118.40(8) C1 O2 H2 . 109.5 HA N HB . 109.5 HA N HC . 109.5 HB N HC . 109.5 C4 N HA . 109.5 C4 N HB . 109.5 C4 N HC . 109.5 N C4 H4A . 109.6 N C4 H4B . 109.6 N C4 C5 . 110.14(8) H4A C4 H4B . 108.1 C5 C4 H4A . 109.6 C5 C4 H4B . 109.6 C4 C5 H5A . 109.5 C4 C5 H5B . 109.5 C4 C5 H5C . 109.5 H5A C5 H5B . 109.5 H5A C5 H5C . 109.5 H5B C5 H5C . 109.5 O5 C3 C3 5_656 111.32(10) O6 C3 C3 5_656 121.50(11) O6 C3 O5 . 127.18(9) C3 O5 H5 . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 O1 . 1.2141(12) C1 C2 . 1.5570(13) C1 O2 . 1.3090(11) C2 O3 . 1.2415(11) C2 O4 . 1.2565(12) O2 H2 . 0.8400 N HA . 0.9100 N HB . 0.9100 N HC . 0.9100 N C4 . 1.4940(12) C4 H4A . 0.9900 C4 H4B . 0.9900 C4 C5 . 1.5122(14) C5 H5A . 0.9800 C5 H5B . 0.9800 C5 H5C . 0.9800 C3 C3 5_656 1.5467(18) C3 O5 . 1.3016(12) C3 O6 . 1.2121(12) O5 H5 . 0.8400 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 O2 H2 O3 6_556 0.84 1.74 2.5717(9) 172.6 yes N HA O4 . 0.91 1.94 2.8472(11) 177.4 yes N HB O1 4_655 0.91 2.04 2.9409(11) 171.9 yes N HC O6 2_655 0.91 2.16 3.0400(10) 163.1 yes O5 H5 O4 . 0.84 1.68 2.5139(10) 173.1 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 O1 C1 C2 O3 -11.28(13) O1 C1 C2 O4 169.03(9) O2 C1 C2 O3 168.94(8) O2 C1 C2 O4 -10.75(12) _cod_database_fobs_code 1551061