#------------------------------------------------------------------------------ #$Date: 2022-08-19 02:41:15 +0100 (Fri, 19 Aug 2022) $ #$Revision: 277316 $ #$URL: svn://www.crystallography.net/cod/cif/2/24/41/2244147.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_2244147 loop_ _publ_author_name 'Nchioua, Intissar' 'Alsubari, Abdulsalam' 'Mague, Joel T.' 'Ramli, Youssef' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of N-(2,6-dimethylphenyl)-2-[3-hydroxy-2-oxo-3-(2-oxopropyl)indolin-1-yl]acetamide ; _journal_coeditor_code ZN2021 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first ; ; _journal_paper_doi 10.1107/S2056989022007848 _journal_volume 78 _journal_year 2022 _chemical_formula_iupac 'C21 H22 N2 O4' _chemical_formula_moiety 'C21 H22 N2 O4' _chemical_formula_sum 'C21 H22 N2 O4' _chemical_formula_weight 366.40 _chemical_name_systematic ; N-(2,6-dimethylphenyl)-2-[3-hydroxy-2-oxo-3-(2-oxopropyl)indolin-\ 1-yl]acetamide ; _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 mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/1 _cell_angle_alpha 90 _cell_angle_beta 98.4680(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.8608(5) _cell_length_b 8.8352(3) _cell_length_c 15.5411(6) _cell_measurement_reflns_used 9714 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 32.6429 _cell_measurement_theta_min 2.9718 _cell_volume 1882.46(12) _computing_cell_refinement ; SAINT (Bruker, 2021) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2021) ; _computing_molecular_graphics ; DIAMOND (Brandenburg & Putz, 2012) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018/1 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON 3 diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_unetI/netI 0.0168 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 101980 _diffrn_reflns_theta_full 32.000 _diffrn_reflns_theta_max 32.641 _diffrn_reflns_theta_min 2.972 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.50 _diffrn_source_voltage 50 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 776 _exptl_crystal_size_max 0.460 _exptl_crystal_size_mid 0.369 _exptl_crystal_size_min 0.260 _refine_diff_density_max 0.418 _refine_diff_density_min -0.313 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 6815 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0450 _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^)+(0.0697P)^2^+0.4122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1205 _refine_ls_wR_factor_ref 0.1285 _reflns_number_gt 5846 _reflns_number_total 6815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file zn2021sup1.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2244147 _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 0.960 _shelx_estimated_absorpt_t_max 0.977 _shelx_hkl_file ; -2 0 0 728.73 20.90 -2 0 0 697.03 20.70 2 0 0 761.72 20.80 -2 0 0 721.73 20.00 -2 0 0 657.33 20.00 2 0 0 735.23 20.00 2 0 0 745.13 20.10 -2 0 0 756.12 20.80 2 0 0 745.13 20.80 -2 0 0 665.33 19.90 2 0 0 758.22 20.00 -2 0 0 669.83 19.40 -2 0 0 679.03 19.40 -2 0 0 751.22 20.10 -2 0 0 664.63 20.00 2 0 0 740.03 20.20 2 0 0 757.62 20.30 2 0 0 729.23 20.90 -2 0 0 727.53 20.30 2 0 0 742.13 20.90 6 0 0 3516.55 92.49 6 0 0 3411.36 91.99 6 0 0 3349.26 95.19 6 0 0 3550.84 94.99 -6 0 0 3401.76 90.59 -6 0 0 3400.46 90.49 -6 0 0 3455.25 93.49 -6 0 0 3428.16 94.89 -6 0 0 3326.07 94.99 6 0 0 3085.69 94.99 -6 0 0 3511.65 92.79 6 0 0 3432.66 93.39 -6 0 0 3279.17 94.79 6 0 0 3451.55 93.39 -6 0 0 3412.36 95.09 -6 0 0 3418.36 92.39 6 0 0 3409.26 94.89 -6 0 0 3347.36 93.09 -6 0 0 3475.75 92.69 6 0 0 3419.86 92.39 6 0 0 3384.06 93.29 7 0 0 3178.48 88.69 -7 0 0 3153.68 88.29 7 0 0 3153.58 86.29 -7 0 0 3124.89 87.99 7 0 0 3021.60 87.69 7 0 0 3154.08 84.99 7 0 0 3031.30 84.39 7 0 0 3068.99 84.79 -7 0 0 3023.20 85.69 -7 0 0 3166.48 85.49 7 0 0 3151.28 88.99 -7 0 0 3120.79 82.89 -7 0 0 2984.30 87.89 -7 0 0 3119.59 82.79 -7 0 0 3137.09 86.09 7 0 0 3048.50 86.19 -7 0 0 3065.29 84.99 -7 0 0 3063.59 85.19 -7 0 0 3146.29 86.49 7 0 0 3107.29 86.19 7 0 0 3158.48 87.89 -8 0 0 2894.11 79.59 8 0 0 2929.41 79.19 8 0 0 2880.21 83.59 8 0 0 2759.62 78.29 8 0 0 2793.02 80.59 8 0 0 2819.52 78.89 8 0 0 2851.91 82.49 -8 0 0 2861.91 79.49 -8 0 0 3041.10 83.39 8 0 0 2893.91 80.69 8 0 0 3031.40 82.89 -8 0 0 2863.71 76.39 -8 0 0 2711.63 76.49 8 0 0 2832.72 80.59 -8 0 0 3004.60 80.99 -8 0 0 2773.12 80.29 -8 0 0 2906.61 79.19 -8 0 0 2881.61 82.49 -8 0 0 2870.21 80.19 -8 0 0 2705.83 82.39 8 0 0 2799.62 83.09 -9 0 0 129.49 4.90 9 0 0 123.09 8.40 9 0 0 107.59 6.70 9 0 0 126.19 7.40 9 0 0 121.99 9.60 9 0 0 121.99 6.50 -9 0 0 122.39 8.20 -9 0 0 139.19 7.70 9 0 0 125.69 8.20 -9 0 0 115.39 7.20 9 0 0 126.49 8.40 9 0 0 131.49 9.70 -9 0 0 127.69 9.30 -9 0 0 135.39 8.70 -9 0 0 113.59 9.60 -9 0 0 134.29 4.80 -9 0 0 114.19 8.00 9 0 0 114.09 9.60 -9 0 0 124.39 7.10 -10 0 0 1199.48 35.50 10 0 0 1118.69 39.00 10 0 0 1015.40 38.30 10 0 0 1145.19 37.60 -10 0 0 1174.18 39.60 10 0 0 1199.68 35.50 -10 0 0 1206.68 37.30 -10 0 0 1189.98 40.60 10 0 0 1135.29 37.00 10 0 0 1113.29 34.00 10 0 0 1164.18 34.60 -10 0 0 1117.99 37.90 10 0 0 1150.78 40.90 10 0 0 1240.78 39.90 -10 0 0 1147.99 36.60 -10 0 0 1130.69 37.20 -10 0 0 1163.38 35.80 11 0 0 192.18 13.60 -11 0 0 162.38 9.40 -11 0 0 171.68 10.80 -11 0 0 184.58 11.30 11 0 0 180.78 12.00 11 0 0 176.38 10.60 -11 0 0 159.38 10.30 11 0 0 178.38 12.80 11 0 0 178.48 8.50 11 0 0 155.88 10.60 11 0 0 173.78 9.40 -11 0 0 177.28 13.00 -11 0 0 162.08 9.00 -12 0 0 136.59 10.30 -12 0 0 112.89 11.80 12 0 0 137.29 10.60 12 0 0 133.39 12.70 -12 0 0 152.88 10.70 12 0 0 136.79 12.20 12 0 0 148.69 8.90 -12 0 0 129.99 8.20 -12 0 0 131.69 8.80 12 0 0 109.29 13.80 -13 0 0 106.69 14.00 13 0 0 83.69 9.20 -13 0 0 123.49 12.50 13 0 0 96.49 11.20 -13 0 0 103.09 9.60 13 0 0 142.09 13.10 13 0 0 110.59 8.20 -13 0 0 102.09 9.50 14 0 0 1079.99 40.40 14 0 0 1036.30 41.70 -14 0 0 1079.19 43.00 14 0 0 1011.20 37.60 -14 0 0 1032.50 37.30 -14 0 0 1030.10 41.30 -14 0 0 1042.40 37.40 -15 0 0 22.20 6.70 -15 0 0 27.60 8.90 15 0 0 22.60 8.60 -15 0 0 29.30 8.30 15 0 0 37.00 8.20 15 0 0 17.10 6.90 -15 0 0 26.00 6.50 -16 0 0 5.00 6.40 16 0 0 11.70 8.50 -16 0 0 13.30 8.20 -16 0 0 4.20 7.20 -16 0 0 13.80 6.30 16 0 0 10.40 6.90 16 0 0 8.60 8.90 17 0 0 531.95 31.30 -17 0 0 563.84 26.70 -17 0 0 569.54 32.20 -17 0 0 609.94 31.70 17 0 0 546.45 30.60 17 0 0 559.14 27.00 18 0 0 18.30 8.60 18 0 0 31.60 8.50 -18 0 0 5.40 5.80 -18 0 0 22.60 9.10 -18 0 0 15.70 9.00 18 0 0 20.40 9.70 19 0 0 212.38 20.80 -19 0 0 212.38 21.00 19 0 0 187.18 18.60 19 0 0 198.38 16.40 -19 0 0 236.68 21.20 -19 0 0 213.88 17.30 20 0 0 120.89 15.60 20 0 0 45.80 16.30 -20 0 0 83.59 15.20 -20 0 0 90.29 15.90 0 -1 0 2.10 0.70 0 -1 0 2.20 0.70 0 -1 0 2.10 0.70 0 -1 0 2.30 0.60 0 -1 0 3.30 0.80 0 1 0 1.20 0.50 0 1 0 4.30 0.90 0 1 0 5.10 1.00 0 1 0 2.30 0.70 5 1 0 4772.92 127.29 5 1 0 4732.03 129.99 -5 1 0 4878.71 132.79 -6 -1 0 5265.47 142.79 6 -1 0 5261.67 141.89 6 -1 0 5026.70 138.49 -6 -1 0 5163.08 142.49 -6 -1 0 5205.58 142.19 6 1 0 5108.79 140.39 6 1 0 5360.96 142.89 6 1 0 5273.27 141.89 -6 1 0 5282.67 142.89 -6 1 0 5196.28 142.69 6 1 0 5242.88 138.39 -8 -1 0 1045.40 32.20 8 -1 0 1001.40 29.40 -8 -1 0 1027.40 33.20 8 -1 0 1026.50 33.90 8 -1 0 1024.90 32.40 -8 -1 0 1084.59 32.90 -8 -1 0 1061.99 33.90 -8 -1 0 1052.19 33.10 8 -1 0 1067.69 35.50 -8 -1 0 992.00 34.50 -8 -1 0 1017.90 34.90 -8 -1 0 1073.09 30.60 8 -1 0 1025.70 34.50 -8 -1 0 1054.09 28.90 8 -1 0 1052.09 32.30 -8 -1 0 1058.39 28.90 -8 -1 0 1041.60 34.20 8 -1 0 1073.79 32.40 8 -1 0 1036.20 29.70 8 1 0 968.40 34.30 8 1 0 1026.60 31.60 -8 1 0 1061.29 30.50 8 1 0 1022.20 34.30 -8 1 0 1003.30 34.60 -8 1 0 1018.40 31.70 8 1 0 1071.79 35.60 -8 1 0 1021.70 34.50 -8 1 0 1020.30 30.20 8 1 0 1078.39 30.30 -8 1 0 1011.80 32.40 8 1 0 996.70 33.30 8 1 0 990.60 34.80 8 1 0 1046.00 33.10 -8 1 0 1039.50 29.60 -8 1 0 1049.79 31.90 -8 1 0 978.10 33.90 9 -1 0 1942.01 60.99 9 -1 0 1852.71 62.19 9 -1 0 1898.71 53.89 -9 -1 0 1982.80 60.59 9 -1 0 1961.00 57.39 -9 -1 0 2048.99 53.19 9 -1 0 2020.00 60.49 -9 -1 0 2021.40 53.19 -9 -1 0 1999.20 59.39 9 -1 0 1950.10 54.09 9 -1 0 1976.20 57.59 -9 -1 0 1953.80 57.09 -9 -1 0 2040.60 57.89 -9 -1 0 2005.90 60.49 -9 -1 0 2017.10 57.29 -9 -1 0 1954.80 58.49 -9 -1 0 2049.49 61.29 9 -1 0 1896.11 57.19 -9 1 0 2055.79 62.09 -9 1 0 1962.80 57.79 -9 1 0 1961.20 55.19 9 1 0 2021.00 61.19 -9 1 0 1977.40 57.29 9 1 0 2083.29 60.39 9 1 0 2040.20 55.09 -9 1 0 1948.71 57.09 -9 1 0 2012.60 57.19 9 1 0 1847.42 58.49 9 1 0 1936.71 58.69 9 1 0 1980.40 58.79 -9 1 0 1795.62 59.49 9 1 0 1926.01 60.29 -9 1 0 1944.01 60.19 -9 1 0 1908.01 54.89 9 1 0 1953.70 57.69 9 1 0 1928.31 56.39 9 1 0 1991.80 61.39 -9 1 0 1935.91 53.99 -9 1 0 1943.81 60.59 10 -1 0 1572.14 48.20 10 -1 0 1631.54 51.49 -10 -1 0 1599.24 46.00 -10 -1 0 1648.34 49.50 10 -1 0 1560.04 48.00 -10 -1 0 1629.14 52.49 -10 -1 0 1613.44 48.40 10 -1 0 1570.54 48.40 10 -1 0 1535.35 44.10 -10 -1 0 1616.44 50.09 10 -1 0 1474.95 43.80 10 -1 0 1550.14 51.89 -10 -1 0 1665.83 49.90 -10 -1 0 1588.74 50.79 -10 1 0 1528.75 45.00 10 1 0 1657.33 45.60 -10 1 0 1565.24 47.90 10 1 0 1561.84 49.40 -10 1 0 1622.94 51.29 10 1 0 1712.63 51.49 10 1 0 1699.33 52.69 -10 1 0 1626.74 52.89 -10 1 0 1483.85 47.10 10 1 0 1688.83 52.99 -10 1 0 1525.15 48.20 -10 1 0 1585.24 45.40 -10 1 0 1584.74 44.00 -10 1 0 1575.34 51.09 10 1 0 1571.84 52.49 -10 1 0 1589.74 48.00 10 1 0 1525.25 49.20 -10 1 0 1528.25 47.60 11 -1 0 0.40 3.50 11 -1 0 6.10 3.40 11 -1 0 16.90 5.60 11 -1 0 3.10 1.80 -11 -1 0 4.30 3.00 -11 -1 0 3.90 4.00 11 -1 0 2.50 3.70 -11 -1 0 4.70 3.40 -11 -1 0 5.90 3.70 -11 -1 0 8.60 4.90 -11 -1 0 6.30 2.90 11 -1 0 -2.70 4.00 -11 1 0 18.70 4.70 -11 1 0 1.80 3.40 -11 1 0 5.80 3.30 -11 1 0 10.10 5.20 11 1 0 -4.70 4.50 11 1 0 8.10 3.70 -11 1 0 -2.60 5.20 11 1 0 2.90 2.80 11 1 0 7.20 3.90 11 1 0 8.70 5.10 -11 1 0 -4.90 2.90 11 1 0 2.00 3.70 11 1 0 6.70 5.70 11 1 0 16.10 4.90 -11 1 0 7.30 2.10 -11 1 0 10.50 2.10 -11 1 0 2.60 2.40 -12 -1 0 339.17 16.40 -12 -1 0 286.27 18.20 12 -1 0 280.97 17.40 -12 -1 0 303.07 15.70 12 -1 0 286.07 15.10 12 -1 0 295.07 15.40 12 -1 0 279.47 17.70 -12 -1 0 334.57 17.10 12 -1 0 312.67 14.80 12 1 0 325.27 16.70 -12 1 0 270.07 14.60 -12 1 0 290.77 14.50 -12 1 0 283.27 14.20 -12 1 0 259.47 14.50 -12 1 0 318.37 16.70 12 1 0 300.47 16.00 12 1 0 302.57 18.40 -12 1 0 283.97 18.60 12 1 0 315.37 18.00 -12 1 0 281.77 17.50 12 1 0 298.27 12.30 13 -1 0 40.10 8.70 -13 -1 0 23.30 6.20 13 -1 0 34.50 8.20 13 -1 0 30.70 5.70 -13 -1 0 24.10 7.70 -13 -1 0 18.70 6.30 13 -1 0 35.50 6.40 -13 1 0 30.00 6.10 -13 1 0 32.50 8.20 13 1 0 17.20 6.70 13 1 0 18.50 6.70 -13 1 0 38.10 6.70 13 1 0 13.70 5.20 -13 1 0 10.60 6.50 -13 1 0 19.20 8.00 -14 -1 0 88.79 11.80 14 -1 0 117.29 12.50 -14 -1 0 107.79 10.60 14 -1 0 84.99 9.40 14 -1 0 95.49 8.80 14 -1 0 95.29 12.50 -14 -1 0 83.09 10.30 14 1 0 94.29 12.20 -14 1 0 81.09 8.60 14 1 0 80.29 9.70 14 1 0 100.99 12.00 -14 1 0 87.29 11.40 -14 1 0 91.49 12.60 -14 1 0 85.29 9.20 15 -1 0 65.99 9.20 -15 -1 0 64.79 12.80 -15 -1 0 55.89 10.70 -15 -1 0 54.09 9.60 15 -1 0 70.39 12.10 15 -1 0 79.49 11.20 -15 -1 0 80.89 10.00 -15 1 0 59.49 13.40 15 1 0 61.49 10.40 -15 1 0 61.79 11.50 15 1 0 64.39 9.50 -15 1 0 75.59 12.30 -15 1 0 76.49 9.30 15 1 0 72.39 11.90 16 -1 0 46.90 8.90 -16 -1 0 53.59 12.60 -16 -1 0 35.80 10.10 16 -1 0 40.10 9.80 16 -1 0 33.90 9.50 -16 -1 0 61.69 10.70 16 1 0 40.10 10.00 -16 1 0 64.69 12.50 -16 1 0 31.30 9.00 -16 1 0 50.19 8.80 16 1 0 54.09 14.20 16 1 0 20.90 8.20 -17 -1 0 20.40 9.40 17 -1 0 36.70 10.20 -17 -1 0 32.70 10.80 -17 -1 0 46.30 11.10 17 -1 0 49.40 11.60 17 -1 0 35.90 7.90 -17 -1 0 29.20 7.70 17 1 0 22.60 8.20 -17 1 0 26.60 10.10 17 1 0 15.60 8.00 -17 1 0 40.80 10.50 -17 1 0 31.90 7.60 18 -1 0 -2.20 6.00 -18 -1 0 16.00 10.30 18 -1 0 10.60 6.20 18 -1 0 7.70 8.20 -18 -1 0 2.70 5.70 -18 -1 0 4.30 7.40 18 1 0 -3.00 6.10 -18 1 0 5.00 7.40 -18 1 0 6.50 7.70 -18 1 0 -3.50 4.50 18 1 0 -8.80 5.60 18 1 0 3.40 5.80 19 -1 0 49.30 9.90 -19 -1 0 38.90 12.60 19 -1 0 46.10 12.00 -19 -1 0 45.30 10.10 -19 -1 0 38.80 11.50 19 -1 0 30.20 11.60 -19 1 0 43.80 11.50 19 1 0 30.80 8.90 19 1 0 42.00 11.00 19 1 0 31.00 10.50 -19 1 0 40.30 8.90 -19 1 0 54.99 13.60 -20 -1 0 21.40 10.30 -20 -1 0 23.00 11.10 20 -1 0 21.30 9.60 -20 1 0 46.80 12.20 -20 1 0 17.30 10.10 20 1 0 9.70 8.80 -1 -2 0 118.99 5.80 -1 -2 0 122.79 5.70 -1 -2 0 114.59 5.70 1 -2 0 123.79 5.50 -1 -2 0 115.39 5.10 -1 -2 0 120.39 6.10 -1 -2 0 119.19 4.90 1 -2 0 132.79 6.10 -1 -2 0 128.59 5.90 1 -2 0 129.39 5.40 1 -2 0 131.89 5.40 -1 -2 0 124.99 6.20 -1 -2 0 119.49 5.90 -1 -2 0 118.79 5.20 1 -2 0 135.89 6.10 -1 -2 0 116.59 5.80 1 -2 0 123.69 6.10 1 -2 0 134.39 5.60 1 2 0 112.29 4.80 -1 2 0 128.29 5.50 1 2 0 122.69 5.10 -1 2 0 132.59 6.10 1 2 0 125.99 5.90 -1 2 0 129.29 5.90 -1 2 0 133.79 5.60 1 2 0 116.79 6.00 1 2 0 110.79 5.10 -1 2 0 138.79 5.60 1 2 0 116.59 5.70 1 2 0 118.99 5.90 1 2 0 118.39 5.80 -1 2 0 125.79 5.50 -1 2 0 131.29 5.90 -1 2 0 121.89 5.90 1 2 0 122.99 5.90 -1 2 0 123.89 5.30 -1 2 0 132.59 5.60 -1 2 0 132.09 6.30 -4 -2 0 1223.98 35.80 4 -2 0 1191.58 34.10 4 -2 0 1210.08 33.20 -4 -2 0 1229.18 36.00 4 -2 0 1177.38 32.90 -4 -2 0 1167.98 36.10 4 -2 0 1220.58 34.30 4 -2 0 1209.48 34.70 4 -2 0 1187.58 34.10 4 -2 0 1225.28 36.20 4 -2 0 1285.27 35.90 -4 -2 0 1195.18 35.40 -4 -2 0 1213.38 34.20 -4 -2 0 1206.58 35.70 -4 -2 0 1041.10 35.20 -4 -2 0 1141.29 35.80 4 -2 0 1214.98 33.10 -4 -2 0 1199.18 36.30 -4 -2 0 1178.28 35.50 4 2 0 1184.58 36.20 -4 2 0 1222.78 34.00 -4 2 0 1234.08 35.70 -4 2 0 1234.08 33.40 -4 2 0 1241.48 33.60 4 2 0 1219.88 36.00 -4 2 0 1190.38 33.90 4 2 0 1172.88 36.00 4 2 0 1223.68 35.80 -4 2 0 1233.38 36.30 4 2 0 1179.58 32.50 4 2 0 1225.08 35.40 4 2 0 1148.79 35.50 -4 2 0 1088.79 33.10 -4 2 0 1185.88 36.30 4 2 0 1164.58 35.60 -4 2 0 1168.98 34.20 4 2 0 1203.48 35.60 -4 2 0 1236.78 36.10 4 2 0 1158.68 34.10 4 2 0 1152.78 32.60 4 2 0 1181.58 35.90 -4 2 0 1242.48 36.30 -4 2 0 1130.29 34.40 -5 -2 0 729.83 22.10 5 -2 0 805.32 25.70 5 -2 0 810.52 26.40 -5 -2 0 786.42 23.80 -5 -2 0 711.73 25.30 5 -2 0 770.32 22.50 -5 -2 0 796.62 25.70 -5 -2 0 815.72 25.80 5 -2 0 811.62 22.50 5 -2 0 843.82 24.60 -5 -2 0 814.42 25.70 5 -2 0 784.92 24.70 5 -2 0 805.52 24.10 -5 -2 0 837.82 26.10 -5 -2 0 833.42 26.60 5 -2 0 801.22 24.20 -5 -2 0 787.02 26.40 -5 -2 0 818.12 26.60 5 2 0 861.61 26.90 -5 2 0 789.92 23.20 5 2 0 786.42 26.10 -5 2 0 787.92 23.20 -5 2 0 790.02 26.40 5 2 0 794.62 26.10 -5 2 0 758.02 26.00 -5 2 0 799.02 24.80 -5 2 0 778.82 26.40 -5 2 0 779.62 23.80 5 2 0 805.32 25.90 -5 2 0 810.42 23.10 5 2 0 838.32 26.30 -5 2 0 782.22 25.50 5 2 0 771.82 25.90 -5 2 0 817.52 26.30 5 2 0 800.32 25.30 5 2 0 798.72 26.00 5 2 0 789.52 23.80 -5 2 0 790.62 23.90 -5 2 0 808.82 23.00 5 2 0 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102.09 7.90 2 -5 0 107.29 8.10 -2 -5 0 111.29 8.00 -2 -5 0 118.09 8.20 -2 -5 0 101.29 6.80 -2 -5 0 118.49 8.40 2 -5 0 99.49 7.00 2 -5 0 107.39 7.10 -2 5 0 108.99 7.90 -2 5 0 99.09 8.10 -2 5 0 99.29 8.40 -2 5 0 99.49 7.10 -2 5 0 94.89 7.70 -2 5 0 105.99 7.90 2 5 0 113.19 8.20 2 5 0 119.59 8.20 -2 5 0 111.89 7.30 2 5 0 100.49 8.00 -2 5 0 112.19 7.60 2 5 0 105.49 8.20 2 5 0 114.39 8.20 2 5 0 100.29 8.50 2 5 0 108.29 6.90 -2 5 0 100.19 7.20 -2 5 0 128.59 7.70 2 5 0 97.89 8.00 2 5 0 106.19 6.80 -2 5 0 102.19 6.90 3 -5 0 433.96 16.30 3 -5 0 409.66 18.50 3 -5 0 389.16 16.90 -3 -5 0 456.75 18.30 3 -5 0 413.76 16.60 -3 -5 0 438.36 19.10 3 -5 0 420.86 18.10 3 -5 0 439.06 16.20 -3 -5 0 438.16 16.10 -3 -5 0 404.06 18.50 -3 -5 0 442.56 18.20 -3 -5 0 449.56 18.00 3 -5 0 476.95 18.80 -3 -5 0 448.76 18.10 -3 -5 0 445.26 18.60 3 -5 0 398.86 18.80 -3 -5 0 447.06 16.20 -3 5 0 442.76 18.50 3 5 0 435.96 18.20 -3 5 0 446.36 16.20 3 5 0 449.36 18.10 -3 5 0 441.16 16.90 3 5 0 446.06 19.10 -3 5 0 417.36 16.90 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18.80 4.60 5 -5 0 26.90 4.00 5 -5 0 9.80 4.30 5 -5 0 15.50 4.80 -5 -5 0 16.20 4.80 -5 -5 0 21.90 4.60 -5 -5 0 27.40 5.30 5 -5 0 16.70 3.80 -5 -5 0 19.90 4.50 5 -5 0 14.10 3.80 -5 -5 0 23.00 5.00 5 -5 0 15.70 3.40 -5 -5 0 12.90 5.10 -5 -5 0 14.20 4.10 -5 -5 0 20.90 4.60 -5 -5 0 26.00 6.00 5 -5 0 22.30 3.80 5 5 0 7.50 4.10 5 5 0 22.40 4.60 -5 5 0 16.20 2.10 -5 5 0 9.80 6.80 5 5 0 26.50 3.60 -5 5 0 4.70 4.00 5 5 0 13.10 3.70 5 5 0 16.60 4.30 -5 5 0 13.10 4.50 5 5 0 25.80 5.40 -5 5 0 23.60 5.20 -5 5 0 16.40 2.50 5 5 0 22.60 5.00 5 5 0 14.10 3.80 5 5 0 16.50 4.40 -5 5 0 16.40 3.50 -5 5 0 17.00 3.80 -5 5 0 17.70 3.90 5 5 0 18.20 3.40 -5 5 0 25.10 5.20 -5 5 0 13.80 3.10 5 5 0 15.70 5.00 -6 -5 0 299.87 14.60 6 -5 0 286.07 11.00 -6 -5 0 271.37 14.50 6 -5 0 285.57 14.40 6 -5 0 299.07 17.60 -6 -5 0 319.07 15.90 -6 -5 0 292.87 15.20 6 -5 0 290.27 11.20 -6 -5 0 288.27 14.90 -6 -5 0 302.37 14.00 -6 -5 0 261.17 15.00 6 -5 0 288.07 11.40 6 5 0 305.47 18.70 -6 5 0 284.07 13.00 -6 5 0 296.97 11.40 -6 5 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1391.96 42.70 8 -5 0 1411.06 46.10 -8 -5 0 1338.27 44.50 -8 -5 0 1305.47 45.30 -8 -5 0 1249.57 44.80 8 -5 0 1349.47 46.40 8 -5 0 1378.56 44.00 -8 -5 0 1426.56 48.70 -8 -5 0 1379.86 45.80 -8 -5 0 1282.67 46.70 -8 -5 0 1356.86 46.30 -8 -5 0 1352.76 42.50 8 -5 0 1378.86 42.50 -8 5 0 1297.97 40.00 8 5 0 1365.36 47.00 -8 5 0 1349.36 43.40 -8 5 0 1359.86 38.70 8 5 0 1336.27 45.70 8 5 0 1337.97 45.00 8 5 0 1312.87 42.50 -8 5 0 1390.26 47.30 -8 5 0 1316.57 46.10 8 5 0 1237.48 44.00 -8 5 0 1376.46 42.40 -8 5 0 1344.67 42.10 -8 5 0 1412.66 41.10 8 5 0 1335.87 46.40 9 -5 0 779.12 30.60 -9 -5 0 706.53 31.20 -9 -5 0 817.62 31.20 -9 -5 0 764.92 34.30 9 -5 0 760.62 27.20 -9 -5 0 777.62 31.90 9 -5 0 762.52 27.30 9 -5 0 763.52 28.40 -9 -5 0 730.63 30.30 -9 -5 0 773.92 27.00 9 -5 0 776.42 31.20 9 5 0 783.52 30.00 9 5 0 745.93 29.80 -9 5 0 782.92 23.50 -9 5 0 765.52 27.20 9 5 0 770.42 31.60 -9 5 0 797.02 27.20 -9 5 0 759.82 26.40 -9 5 0 794.72 31.60 -9 5 0 700.93 25.40 -9 5 0 745.53 31.70 -9 5 0 749.62 27.90 10 -5 0 90.59 11.20 -10 -5 0 106.39 11.10 10 -5 0 94.89 9.30 10 -5 0 101.29 8.50 -10 -5 0 97.59 8.10 -10 -5 0 81.49 11.60 10 -5 0 92.09 11.00 -10 -5 0 110.19 11.50 -10 5 0 105.79 8.60 10 5 0 99.59 10.80 -10 5 0 94.19 11.60 -10 5 0 103.49 8.40 -10 5 0 80.29 8.50 10 5 0 119.19 11.10 -10 5 0 88.29 5.40 10 5 0 108.29 11.80 10 5 0 115.59 11.50 -10 5 0 105.89 11.90 -10 5 0 97.19 8.50 -11 -5 0 119.79 8.70 -11 -5 0 159.38 14.10 11 -5 0 141.59 13.10 -11 -5 0 138.09 14.00 11 -5 0 127.59 9.60 11 -5 0 137.29 10.60 11 -5 0 119.89 12.10 -11 -5 0 127.89 12.40 -11 5 0 110.59 9.30 -11 5 0 123.79 10.10 11 5 0 134.29 12.70 -11 5 0 134.19 13.50 11 5 0 151.28 12.70 11 5 0 131.89 12.20 -11 5 0 130.39 10.40 11 5 0 117.29 12.70 -11 5 0 110.49 12.90 12 -5 0 2.00 4.10 -12 -5 0 4.30 5.20 -12 -5 0 4.60 6.80 12 -5 0 4.20 5.90 -12 -5 0 3.10 5.80 12 -5 0 1.80 4.70 12 -5 0 -6.70 2.60 12 5 0 1.90 5.00 -12 5 0 7.40 4.00 12 5 0 -7.60 4.60 -12 5 0 4.80 6.10 -12 5 0 5.30 6.20 12 5 0 4.30 5.30 -12 5 0 2.00 5.30 -13 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225.58 12.40 1 -6 0 229.88 13.40 -1 -6 0 239.08 12.30 -1 -6 0 248.68 11.70 -1 -6 0 274.47 14.00 -1 -6 0 264.67 13.70 -1 -6 0 245.48 9.40 1 -6 0 267.77 13.40 1 -6 0 261.97 11.90 1 -6 0 223.78 12.90 1 -6 0 222.18 13.30 -1 -6 0 253.27 13.20 1 6 0 250.47 11.60 1 6 0 257.17 13.80 1 6 0 245.58 14.30 1 6 0 249.08 13.60 1 6 0 259.67 13.80 -1 6 0 253.67 12.50 -1 6 0 253.27 14.40 1 6 0 250.77 13.20 1 6 0 244.88 12.30 -1 6 0 241.98 13.50 -1 6 0 248.28 12.90 1 6 0 255.37 15.10 -1 6 0 257.67 12.90 -1 6 0 222.68 12.50 -1 6 0 237.18 13.10 1 6 0 241.48 13.30 -1 6 0 234.78 12.70 -1 6 0 237.48 12.50 -1 6 0 235.68 13.70 -1 6 0 240.18 13.80 1 6 0 257.17 13.80 -2 -6 0 1503.25 49.20 -2 -6 0 1587.44 49.70 2 -6 0 1558.74 47.60 2 -6 0 1431.66 48.30 -2 -6 0 1599.84 49.99 -2 -6 0 1531.75 48.70 -2 -6 0 1574.84 49.40 2 -6 0 1593.74 47.40 -2 -6 0 1614.64 44.90 -2 -6 0 1465.95 46.40 -2 -6 0 1454.05 48.20 2 -6 0 1506.65 48.90 2 -6 0 1539.15 49.60 2 -6 0 1531.85 48.40 -2 -6 0 1609.14 50.39 2 -6 0 1469.75 46.50 2 -6 0 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470.25 24.50 -8 7 0 449.76 24.30 -8 7 0 485.85 23.60 -8 7 0 465.35 20.60 8 7 0 449.66 21.10 9 -7 0 -1.50 5.00 -9 -7 0 4.60 5.70 -9 -7 0 2.90 5.00 9 -7 0 2.90 4.10 -9 -7 0 -1.80 3.90 -9 -7 0 3.60 6.60 9 -7 0 2.80 4.70 -9 7 0 0.10 5.30 -9 7 0 4.80 3.90 -9 7 0 9.10 6.40 9 7 0 6.60 6.00 9 7 0 -7.50 4.00 9 7 0 2.70 4.50 9 7 0 -5.70 4.60 -10 -7 0 237.88 16.90 10 -7 0 227.98 14.20 -10 -7 0 271.97 19.70 -10 -7 0 249.58 17.70 10 -7 0 241.58 17.50 -10 -7 0 243.28 14.60 10 -7 0 259.37 16.30 10 7 0 234.68 16.00 -10 7 0 232.58 14.30 -10 7 0 229.88 18.10 -10 7 0 207.28 18.40 10 7 0 229.58 18.00 10 7 0 234.78 17.70 10 7 0 227.18 16.40 11 -7 0 -4.70 4.80 -11 -7 0 -0.10 3.90 11 -7 0 2.30 4.70 11 -7 0 -1.70 3.70 -11 -7 0 0.00 4.80 -11 -7 0 1.10 6.20 -11 -7 0 -7.90 4.30 -11 7 0 2.50 5.50 11 7 0 -0.40 4.90 11 7 0 -7.10 4.20 -11 7 0 -4.50 3.00 -11 7 0 2.20 5.90 11 7 0 -2.10 5.70 -12 -7 0 -1.60 4.90 12 -7 0 1.50 3.70 -12 -7 0 -5.40 6.70 12 -7 0 -5.00 5.50 -12 -7 0 -3.50 5.60 12 7 0 -2.10 5.50 -12 7 0 3.20 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2 124.19 9.50 -4 -4 2 97.89 7.30 4 -4 -2 86.99 4.40 -4 -4 2 77.89 6.70 -4 -4 2 92.89 7.30 -4 4 2 75.09 7.30 4 4 -2 86.29 7.30 -4 4 2 78.69 7.50 -4 4 2 92.09 6.50 4 4 -2 89.29 7.40 4 4 -2 86.59 5.80 4 4 -2 85.99 7.50 -4 4 2 88.69 7.00 4 4 -2 96.19 6.90 -4 4 2 96.39 7.20 4 4 -2 75.59 7.30 -4 4 2 99.79 7.50 4 4 -2 87.49 7.40 4 4 -2 97.49 6.40 -4 4 2 95.79 6.70 4 4 -2 93.89 7.20 -4 4 2 79.09 6.30 -4 4 2 84.89 6.70 4 4 -2 98.59 7.60 -4 4 2 86.09 4.70 4 4 -2 91.59 5.70 4 4 -2 101.59 6.80 -4 4 2 86.99 4.50 -3 -4 2 674.73 23.60 -3 -4 2 669.83 23.70 3 -4 -2 707.03 23.80 3 -4 -2 693.53 24.40 -3 -4 2 662.83 24.10 -3 -4 2 657.03 23.80 -3 -4 2 665.23 23.90 3 -4 -2 667.43 20.80 -3 -4 2 666.93 24.50 3 -4 -2 692.83 23.90 3 -4 -2 699.83 23.70 -3 -4 2 683.93 22.50 3 -4 -2 669.03 22.80 -3 -4 2 650.43 23.10 3 -4 -2 707.63 23.80 -3 -4 2 666.13 20.90 3 -4 -2 671.43 23.40 -3 -4 2 677.93 23.70 3 4 -2 701.63 22.20 -3 4 2 680.63 23.00 3 4 -2 678.23 24.40 -3 4 2 625.14 22.80 3 4 -2 649.93 23.70 -3 4 2 663.93 23.40 3 4 -2 676.33 24.10 -3 4 2 668.13 20.60 -3 4 2 642.84 23.10 -3 4 2 668.13 23.10 3 4 -2 625.24 23.80 -3 4 2 675.23 24.60 3 4 -2 667.33 20.80 3 4 -2 674.33 24.00 3 4 -2 660.23 23.00 3 4 -2 677.13 22.00 3 4 -2 698.63 22.70 -3 4 2 653.43 23.50 -3 4 2 686.13 23.30 -3 4 2 623.64 24.00 3 4 -2 685.73 24.00 -3 4 2 669.83 19.30 3 4 -2 689.33 25.70 2 -4 -2 3084.49 85.39 -2 -4 2 2954.20 81.89 -2 -4 2 3016.60 85.29 2 -4 -2 3052.39 83.09 -2 -4 2 3008.60 84.99 2 -4 -2 2955.40 84.69 -2 -4 2 3083.69 85.69 2 -4 -2 2885.31 84.99 2 -4 -2 3067.09 85.59 -2 -4 2 2960.80 85.79 -2 -4 2 3080.69 85.19 -2 -4 2 3011.90 85.39 2 -4 -2 3054.49 85.59 2 -4 -2 2952.90 80.59 -2 -4 2 3080.49 86.39 2 -4 -2 2956.80 85.89 -2 -4 2 3137.09 83.39 -2 -4 2 3087.89 86.09 2 -4 -2 3077.49 85.79 2 4 -2 2983.50 84.39 2 4 -2 2912.11 84.99 -2 4 2 3025.60 85.29 -2 4 2 3081.29 85.39 2 4 -2 3028.70 86.19 -2 4 2 2913.51 85.39 -2 4 2 3070.59 85.29 -2 4 2 3159.68 86.69 -2 4 2 3080.59 85.29 2 4 -2 3111.39 85.89 2 4 -2 3012.80 85.49 2 4 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62.39 3 5 -2 2073.19 61.39 3 5 -2 2157.38 64.09 2 -5 -2 987.30 33.40 -2 -5 2 986.20 29.50 -2 -5 2 1013.80 33.50 -2 -5 2 1013.70 33.90 2 -5 -2 921.91 32.60 -2 -5 2 1000.20 33.60 2 -5 -2 913.91 32.30 2 -5 -2 1016.40 32.40 -2 -5 2 1025.30 33.50 2 -5 -2 999.70 33.60 2 -5 -2 915.11 32.80 2 -5 -2 979.30 31.10 2 -5 -2 995.40 32.60 -2 -5 2 996.80 33.30 -2 -5 2 1043.10 30.60 2 -5 -2 950.00 33.60 -2 -5 2 977.00 32.60 -2 -5 2 995.40 32.60 -2 -5 2 1001.90 34.10 -2 5 2 978.90 34.30 -2 5 2 1010.90 33.00 -2 5 2 984.20 32.70 2 5 -2 998.30 33.10 -2 5 2 1028.10 33.60 -2 5 2 1008.10 33.00 2 5 -2 1012.20 33.30 -2 5 2 1013.20 33.30 -2 5 2 1000.40 33.00 2 5 -2 1009.50 33.60 -2 5 2 969.40 33.00 2 5 -2 1038.00 34.30 -2 5 2 977.10 32.80 2 5 -2 935.61 33.40 2 5 -2 987.70 31.80 2 5 -2 983.60 29.80 2 5 -2 1007.90 33.50 -2 5 2 975.60 30.80 -2 5 2 1009.90 32.60 2 5 -2 999.20 33.00 2 5 -2 1061.09 33.90 2 5 -2 994.00 29.30 -1 -5 2 1995.10 58.89 1 -5 -2 1908.41 59.09 1 -5 -2 2024.30 52.69 1 -5 -2 2031.00 57.99 -1 -5 2 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214.78 21.40 -4 -3 22 6.70 8.60 -4 -3 22 6.40 8.10 4 -3 -22 -6.30 6.50 -4 -3 22 3.50 7.80 4 -3 -22 -10.20 6.40 4 3 -22 -4.80 6.30 -4 3 22 0.70 6.90 4 3 -22 -2.50 8.00 4 3 -22 -1.20 7.40 -4 3 22 4.30 9.20 3 -3 -22 23.70 10.50 3 -3 -22 27.60 10.30 -3 -3 22 40.80 11.40 -3 -3 22 48.10 13.20 -3 -3 22 43.40 11.10 -3 3 22 34.40 11.60 3 3 -22 50.09 12.40 3 3 -22 42.30 11.00 -3 3 22 45.50 12.30 3 3 -22 50.59 14.10 -3 3 22 27.10 10.80 2 -3 -22 8.70 8.00 -2 -3 22 -3.70 6.70 -2 -3 22 -1.30 6.10 2 -3 -22 -4.40 6.10 2 -3 -22 -6.10 6.40 -2 -3 22 9.10 8.70 -2 3 22 3.20 8.40 2 3 -22 9.70 9.20 -2 3 22 -10.60 5.80 -2 3 22 -0.60 6.70 2 3 -22 4.30 6.40 2 3 -22 3.20 7.10 -1 -3 22 49.99 13.00 -1 -3 22 53.99 13.50 -1 -3 22 57.59 11.90 1 -3 -22 50.09 15.20 1 -3 -22 44.00 11.40 1 -3 -22 62.89 12.50 1 -3 -22 52.19 12.50 1 3 -22 44.30 12.40 -1 3 22 50.09 13.60 -1 3 22 37.10 11.90 -1 3 22 57.59 13.40 1 3 -22 25.60 9.00 1 3 -22 38.20 12.10 0 -3 -22 94.99 19.40 0 -3 -22 128.69 16.80 0 -3 22 132.99 17.80 0 -3 -22 135.29 16.50 0 3 -22 97.39 17.20 0 3 22 151.78 18.30 0 3 22 124.19 16.40 -1 -3 -22 -3.00 7.50 1 -3 22 -1.80 5.60 -1 -3 -22 9.80 8.40 1 -3 22 -3.30 10.30 -1 -3 -22 4.20 6.90 1 -3 22 3.60 8.40 -1 3 -22 -7.70 6.70 -1 3 -22 0.40 6.30 1 3 22 13.50 9.70 -1 3 -22 -1.80 8.00 1 3 22 3.40 7.10 1 3 22 -6.10 8.10 2 -3 22 87.39 18.70 2 -3 22 95.19 13.40 -2 -3 -22 77.09 15.50 2 3 22 93.89 16.20 -2 3 -22 90.19 16.50 2 3 22 91.99 18.50 -2 3 -22 102.79 14.00 2 3 22 105.69 16.90 -3 -3 -22 235.78 20.20 -3 3 -22 235.78 23.20 7 -4 -22 16.80 9.70 -7 -4 22 30.40 11.50 7 4 -22 38.60 13.60 -7 4 22 21.70 13.30 6 -4 -22 35.80 12.50 -6 -4 22 35.40 16.50 6 -4 -22 65.89 15.60 -6 -4 22 48.50 11.70 -6 -4 22 45.30 12.00 6 4 -22 43.60 13.00 6 4 -22 60.29 13.50 6 4 -22 39.90 11.40 -6 4 22 55.89 14.50 5 -4 -22 255.97 28.80 5 -4 -22 235.88 24.50 -5 -4 22 213.88 21.00 -5 -4 22 258.77 34.30 -5 -4 22 214.18 27.90 5 4 -22 231.38 23.60 -5 4 22 214.78 22.20 5 4 -22 293.27 23.70 5 4 -22 232.88 21.90 -5 4 22 300.07 31.70 -4 -4 22 149.09 20.40 -4 -4 22 169.38 26.40 4 -4 -22 149.99 18.40 4 4 -22 155.88 20.00 4 4 -22 158.48 18.90 -4 4 22 175.68 20.40 4 4 -22 157.78 20.10 -4 4 22 201.08 22.00 3 -4 -22 37.30 11.30 -3 -4 22 34.20 17.60 -3 -4 22 49.40 17.20 3 4 -22 75.39 19.80 -3 4 22 44.80 13.60 -3 4 22 31.30 11.80 3 4 -22 40.50 14.00 3 4 -22 37.70 12.10 -2 -4 22 36.20 14.90 2 -4 -22 57.59 13.00 -2 -4 22 51.39 15.20 2 -4 -22 50.49 13.60 -2 -4 22 47.60 13.10 -2 4 22 24.10 11.40 -2 4 22 44.20 12.20 2 4 -22 39.80 12.40 1 -4 -22 52.69 13.10 -1 -4 22 64.69 14.20 -1 -4 22 61.89 12.30 -1 -4 22 64.99 19.60 1 4 -22 68.69 15.50 -1 4 22 90.69 16.20 -1 4 22 60.49 12.10 1 4 -22 51.39 11.40 1 4 -22 79.19 15.60 0 -4 22 17.60 9.80 0 -4 22 2.80 6.80 0 -4 -22 16.20 9.60 0 -4 -22 14.20 8.30 0 4 -22 1.70 6.30 0 4 -22 2.40 8.50 0 4 22 10.90 7.80 0 4 -22 8.00 8.30 0 4 22 0.60 8.30 0 4 22 6.10 9.10 -1 -4 -22 75.79 17.60 1 -4 22 44.80 13.00 1 -4 22 71.99 12.30 -1 -4 -22 48.40 12.60 -1 -4 -22 71.99 15.10 1 -4 22 63.99 15.90 -1 4 -22 68.39 15.10 1 4 22 53.09 13.20 -1 4 -22 78.19 15.90 -1 4 -22 80.09 13.30 1 4 22 49.99 13.10 -7 0 23 -5.40 7.00 7 0 -23 1.20 9.20 6 0 -23 -4.40 6.80 6 0 -23 5.00 9.50 -6 0 23 8.60 8.90 5 0 -23 0.40 7.90 -5 0 23 4.20 7.80 -5 0 23 -7.90 6.30 5 0 -23 -0.10 8.30 4 0 -23 -0.70 7.50 -4 0 23 1.70 7.10 4 0 -23 -5.80 6.60 -4 0 23 -9.10 5.30 3 0 -23 -4.90 8.70 3 0 -23 8.80 10.30 -3 0 23 -7.40 5.40 3 0 -23 -2.10 6.60 -3 0 23 -0.10 7.20 -2 0 23 2.00 6.90 2 0 -23 -6.40 5.70 2 0 -23 -6.40 6.80 2 0 -23 9.80 8.40 -2 0 23 5.50 8.60 1 0 -23 2.80 8.30 -1 0 23 -6.20 7.20 1 0 -23 -8.80 6.20 -1 0 23 -0.90 7.50 1 0 -23 -8.00 4.90 1 0 -23 -1.50 7.10 0 0 -23 -9.60 6.20 0 0 -23 -12.20 8.00 0 0 23 -1.40 7.50 0 0 23 -0.30 6.90 0 0 -23 -7.60 10.90 0 0 -23 3.20 7.70 -1 0 -23 -5.60 6.60 -1 0 -23 -4.30 7.90 1 0 23 -4.20 5.50 -1 0 -23 -8.40 5.00 1 0 23 -5.00 6.50 -1 0 -23 -3.00 7.60 -7 -1 23 98.49 17.20 7 -1 -23 102.19 17.20 -7 1 23 99.39 17.10 7 1 -23 89.09 16.70 -6 -1 23 87.59 15.10 6 -1 -23 114.19 18.20 6 -1 -23 93.29 15.10 -6 -1 23 72.29 14.20 -6 -1 23 101.49 17.30 6 1 -23 106.59 17.70 -6 1 23 71.69 15.30 6 1 -23 92.29 16.10 -5 -1 23 12.10 9.10 -5 -1 23 9.60 8.10 -5 -1 23 8.60 9.40 5 -1 -23 7.60 9.10 5 -1 -23 6.80 10.40 -5 1 23 4.70 7.60 5 1 -23 4.40 7.80 5 1 -23 23.20 10.60 -5 1 23 6.50 8.70 5 1 -23 -0.40 8.10 -4 -1 23 6.20 7.00 4 -1 -23 5.10 9.70 -4 -1 23 -5.00 7.10 4 1 -23 -0.50 8.80 4 1 -23 19.60 9.90 -4 1 23 15.90 10.00 -4 1 23 7.30 7.50 4 1 -23 15.90 9.20 3 -1 -23 136.59 17.40 -3 -1 23 181.58 19.00 -3 -1 23 153.08 19.70 3 -1 -23 156.38 18.20 3 -1 -23 145.59 21.10 -3 1 23 146.79 17.80 3 1 -23 172.38 18.90 -3 1 23 148.69 19.00 -2 -1 23 32.40 11.40 2 -1 -23 59.59 13.30 2 -1 -23 47.10 11.80 -2 -1 23 44.30 12.40 2 -1 -23 34.50 14.60 2 -1 -23 32.40 11.00 -2 1 23 38.20 11.10 2 1 -23 67.29 14.10 -2 1 23 26.10 11.10 1 -1 -23 88.29 14.90 -1 -1 23 67.89 13.70 1 -1 -23 64.19 13.70 1 -1 -23 70.79 14.40 1 -1 -23 83.59 14.60 -1 1 23 96.79 17.10 1 1 -23 61.49 13.60 1 1 -23 107.99 24.20 -1 1 23 63.69 14.50 0 -1 23 67.99 14.50 0 -1 23 50.79 11.20 0 -1 -23 53.89 13.10 0 -1 -23 63.69 13.20 0 1 -23 53.39 13.90 0 1 -23 59.69 12.30 0 1 -23 105.09 27.30 0 1 23 51.49 13.90 0 1 23 44.30 12.30 0 1 -23 65.59 14.90 -1 -1 -23 13.30 9.10 -1 -1 -23 4.40 8.40 -1 -1 -23 8.20 6.80 -1 -1 -23 2.10 7.90 1 -1 23 -0.40 6.30 1 -1 23 6.40 9.40 -1 1 -23 8.70 8.90 -1 1 -23 3.30 8.50 -1 1 -23 3.90 10.90 1 1 23 -2.00 6.30 -1 1 -23 -2.20 5.70 1 1 23 4.90 8.80 -6 -2 23 -2.30 7.40 6 -2 -23 -5.90 8.80 6 -2 -23 -4.40 7.70 -6 -2 23 9.50 8.90 -6 -2 23 0.50 6.80 6 2 -23 7.80 8.00 -6 2 23 0.80 7.80 6 2 -23 -1.20 7.80 -6 2 23 5.30 8.10 -5 -2 23 -0.70 7.20 -5 -2 23 2.20 9.70 5 -2 -23 1.00 7.40 -5 -2 23 -10.40 5.70 5 2 -23 -10.80 7.70 5 2 -23 8.60 7.50 5 2 -23 -4.20 7.90 -5 2 23 -0.90 7.50 -5 2 23 13.60 8.90 -4 -2 23 52.29 13.30 -4 -2 23 59.59 13.70 4 2 -23 82.39 16.10 -4 2 23 65.59 14.10 -4 2 23 83.89 15.90 -4 2 23 90.89 15.50 4 2 -23 75.29 14.20 3 -2 -23 170.68 25.10 3 -2 -23 151.68 20.70 -3 -2 23 209.28 21.30 3 2 -23 202.58 22.10 3 2 -23 202.48 27.00 -3 2 23 182.38 20.90 -3 2 23 193.58 19.80 -3 2 23 157.28 18.40 2 -2 -23 69.79 13.50 -2 -2 23 76.89 16.10 2 -2 -23 86.69 19.30 2 -2 -23 58.79 13.10 -2 -2 23 50.99 12.90 -2 -2 23 94.79 16.20 2 -2 -23 96.29 16.30 -2 2 23 71.49 14.70 -2 2 23 60.09 14.20 2 2 -23 42.70 15.00 2 2 -23 50.29 13.90 2 2 -23 76.59 15.50 -2 2 23 70.19 13.80 1 -2 -23 9.30 8.90 1 -2 -23 5.70 8.40 -1 -2 23 14.80 8.90 1 -2 -23 17.70 9.30 1 -2 -23 15.20 9.10 -1 -2 23 19.50 8.80 -1 2 23 19.50 11.30 1 2 -23 17.10 9.30 -1 2 23 4.90 8.50 1 2 -23 16.90 8.80 1 2 -23 2.70 8.00 -1 2 23 7.70 8.70 0 -2 -23 35.90 11.80 0 -2 23 63.89 13.90 0 -2 -23 62.19 13.70 0 -2 -23 56.29 15.50 0 -2 23 61.19 13.10 0 2 23 52.19 13.10 0 2 -23 47.40 13.00 0 2 -23 68.19 12.40 0 2 23 60.29 12.90 0 2 -23 57.09 14.30 0 2 23 47.80 13.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 73401 _shelx_res_file ; TITL JTM1529_0m_a.res in P2(1)/c JTM1529_0m_a.res created by SHELXL-2019/1 at 16:16:03 on 31-Mar-2022 REM Old TITL JTM1529_0m in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.140, Rweak 0.004, Alpha 0.030 REM 1.317 for 269 systematic absences, Orientation as input REM Formula found by SHELXT: C21 N2 O4 CELL 0.71073 13.8608 8.8352 15.5411 90.000 98.468 90.000 ZERR 4.000 0.0005 0.0003 0.0006 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O UNIT 84 88 8 16 TEMP -123 SIZE 0.26 0.369 0.46 L.S. 5 BOND $H LIST 4 FMAP 2 PLAN 5 CONF EQIV $1 -x, -y, -z+1 HTAB O1 O2_$1 HTAB N2 O3 EQIV $2 x, -y+1/2, z+1/2 HTAB C9 O4_$2 HTAB C11 O4_$2 EQIV $3 -x, -y+1, -z+1 HTAB C12 O1_$3 MPLA C1 > C6 MPLA C1 C6 C7 C8 N1 MPLA C12 C13 N2 O4 MPLA C14 > C19 ACTA 64 OMIT 2 1 7 WGHT 0.069700 0.412200 FVAR 1.43631 O1 4 -0.016187 0.152402 0.585194 11.00000 0.02139 0.01807 = 0.03198 0.00188 0.00892 -0.00252 H1 2 -0.021128 0.055081 0.581017 11.00000 -1.50000 O2 4 0.066276 0.152749 0.417100 11.00000 0.03237 0.01956 = 0.02124 -0.00406 0.00453 -0.00364 O3 4 0.278917 0.188501 0.550466 11.00000 0.02613 0.03027 = 0.04191 0.01394 0.00786 -0.00009 O4 4 0.207713 0.567740 0.302037 11.00000 0.03026 0.03610 = 0.02064 0.01066 0.00534 0.00040 N1 3 0.106666 0.385673 0.478264 11.00000 0.02299 0.01468 = 0.01621 0.00066 0.00446 -0.00125 N2 3 0.284540 0.437508 0.418235 11.00000 0.02208 0.02416 = 0.02127 0.00691 0.00507 0.00055 H2A 2 0.278036 0.372379 0.459303 11.00000 0.03462 C1 1 0.122854 0.447540 0.563292 11.00000 0.02138 0.01529 = 0.01777 -0.00073 0.00453 -0.00097 C2 1 0.145197 0.595799 0.587166 11.00000 0.02964 0.01571 = 0.02371 -0.00129 0.00624 -0.00325 AFIX 43 H2 2 0.154105 0.670797 0.545243 11.00000 -1.20000 AFIX 0 C3 1 0.154089 0.630262 0.676080 11.00000 0.03477 0.01983 = 0.02657 -0.00621 0.00571 -0.00369 AFIX 43 H3 2 0.169109 0.730952 0.694915 11.00000 -1.20000 AFIX 0 C4 1 0.141337 0.519835 0.737227 11.00000 0.03563 0.02691 = 0.02025 -0.00527 0.00435 -0.00203 AFIX 43 H4 2 0.147813 0.545934 0.797102 11.00000 -1.20000 AFIX 0 C5 1 0.119019 0.370410 0.711260 11.00000 0.03111 0.02259 = 0.01795 0.00077 0.00485 -0.00115 AFIX 43 H5 2 0.110095 0.294882 0.752878 11.00000 -1.20000 AFIX 0 C6 1 0.110280 0.335362 0.623804 11.00000 0.02257 0.01535 = 0.01790 -0.00017 0.00444 -0.00100 C7 1 0.081987 0.189136 0.576604 11.00000 0.02056 0.01453 = 0.01925 0.00122 0.00505 -0.00193 C8 1 0.084727 0.235209 0.480753 11.00000 0.01964 0.01554 = 0.01927 -0.00045 0.00365 -0.00052 C9 1 0.150028 0.056063 0.603962 11.00000 0.02347 0.01568 = 0.02359 0.00289 0.00452 0.00039 AFIX 23 H9A 2 0.147274 0.032787 0.665866 11.00000 -1.20000 H9B 2 0.125732 -0.033851 0.569376 11.00000 -1.20000 AFIX 0 C10 1 0.255016 0.082742 0.592826 11.00000 0.02361 0.02003 = 0.02358 0.00101 0.00442 0.00155 C11 1 0.328613 -0.027777 0.635802 11.00000 0.02713 0.03099 = 0.03739 0.00934 0.00717 0.00814 AFIX 137 H11A 2 0.307193 -0.131044 0.619844 11.00000 -1.50000 H11B 2 0.335063 -0.015875 0.699085 11.00000 -1.50000 H11C 2 0.391777 -0.008787 0.616620 11.00000 -1.50000 AFIX 0 C12 1 0.106659 0.470276 0.398693 11.00000 0.02276 0.01958 = 0.01801 0.00414 0.00426 0.00097 AFIX 23 H12A 2 0.077300 0.570684 0.406183 11.00000 -1.20000 H12B 2 0.063673 0.417265 0.351674 11.00000 -1.20000 AFIX 0 C13 1 0.204970 0.494781 0.368782 11.00000 0.02370 0.01855 = 0.01734 0.00115 0.00442 -0.00029 C14 1 0.379686 0.457885 0.394380 11.00000 0.02149 0.03541 = 0.02302 0.00951 0.00340 -0.00084 C15 1 0.425516 0.333522 0.362567 11.00000 0.02991 0.04776 = 0.03341 0.01356 0.01018 0.01281 C16 1 0.517762 0.356835 0.338359 11.00000 0.03419 0.08529 = 0.05170 0.03130 0.01991 0.02701 AFIX 43 H16 2 0.550264 0.275060 0.315182 11.00000 -1.20000 AFIX 0 C17 1 0.562203 0.497075 0.347694 11.00000 0.02366 0.11026 = 0.06682 0.05026 0.01178 0.00298 AFIX 43 H17 2 0.625396 0.510315 0.332070 11.00000 -1.20000 AFIX 0 C18 1 0.515642 0.617171 0.379361 11.00000 0.03228 0.07970 = 0.05909 0.03318 -0.00196 -0.02115 AFIX 43 H18 2 0.547197 0.712839 0.385442 11.00000 -1.20000 AFIX 0 C19 1 0.422634 0.601623 0.402883 11.00000 0.03283 0.04538 = 0.03418 0.01348 -0.00102 -0.01311 C20 1 0.378031 0.180973 0.355348 11.00000 0.05855 0.03981 = 0.05984 -0.00140 0.02148 0.01587 AFIX 137 H20A 2 0.315758 0.187197 0.316412 11.00000 -1.50000 H20B 2 0.366401 0.147447 0.413048 11.00000 -1.50000 H20C 2 0.420847 0.108401 0.331858 11.00000 -1.50000 AFIX 0 C21 1 0.371712 0.734379 0.436040 11.00000 0.06907 0.03495 = 0.05216 -0.00151 0.00186 -0.01957 AFIX 137 H21A 2 0.322214 0.772932 0.389673 11.00000 -1.50000 H21B 2 0.419331 0.814269 0.454501 11.00000 -1.50000 H21C 2 0.340299 0.702735 0.485625 11.00000 -1.50000 AFIX 0 HKLF 4 REM JTM1529_0m_a.res in P2(1)/c REM wR2 = 0.1285, GooF = S = 1.066, Restrained GooF = 1.066 for all data REM R1 = 0.0450 for 5846 Fo > 4sig(Fo) and 0.0531 for all 6815 data REM 254 parameters refined using 0 restraints END WGHT 0.0696 0.4130 REM Highest difference peak 0.418, deepest hole -0.313, 1-sigma level 0.048 Q1 1 0.1567 0.4831 0.3867 11.00000 0.05 0.42 Q2 1 0.1325 0.5219 0.5733 11.00000 0.05 0.42 Q3 1 0.1214 0.3956 0.5960 11.00000 0.05 0.41 Q4 1 0.2005 0.0747 0.6001 11.00000 0.05 0.40 Q5 1 0.0962 0.2628 0.6044 11.00000 0.05 0.40 ; _shelx_res_checksum 54986 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 O O1 -0.01619(5) 0.15240(7) 0.58519(4) 0.02331(13) Uani d 1 . . H H1 -0.0211(11) 0.0551(17) 0.5810(10) 0.035 Uiso d 1 . . O O2 0.06628(5) 0.15275(7) 0.41710(4) 0.02433(13) Uani d 1 . . O O3 0.27892(5) 0.18850(8) 0.55047(5) 0.03248(16) Uani d 1 . . O O4 0.20771(5) 0.56774(9) 0.30204(4) 0.02884(15) Uani d 1 . . N N1 0.10667(5) 0.38567(7) 0.47826(4) 0.01780(13) Uani d 1 . . N N2 0.28454(5) 0.43751(9) 0.41823(5) 0.02231(14) Uani d 1 . . H H2A 0.2780(10) 0.3724(17) 0.4593(10) 0.035(3) Uiso d 1 . . C C1 0.12285(6) 0.44754(8) 0.56329(5) 0.01798(14) Uani d 1 . . C C2 0.14520(7) 0.59580(9) 0.58717(6) 0.02279(16) Uani d 1 . . H H2 0.154105 0.670797 0.545243 0.027 Uiso calc 1 . . C C3 0.15409(7) 0.63026(10) 0.67608(6) 0.02693(17) Uani d 1 . . H H3 0.169109 0.730952 0.694915 0.032 Uiso calc 1 . . C C4 0.14134(7) 0.51983(11) 0.73723(6) 0.02757(18) Uani d 1 . . H H4 0.147813 0.545934 0.797102 0.033 Uiso calc 1 . . C C5 0.11902(7) 0.37041(10) 0.71126(5) 0.02376(16) Uani d 1 . . H H5 0.110095 0.294882 0.752878 0.029 Uiso calc 1 . . C C6 0.11028(6) 0.33536(9) 0.62380(5) 0.01846(14) Uani d 1 . . C C7 0.08199(6) 0.18914(8) 0.57660(5) 0.01790(14) Uani d 1 . . C C8 0.08473(6) 0.23521(9) 0.48075(5) 0.01807(14) Uani d 1 . . C C9 0.15003(6) 0.05606(9) 0.60396(5) 0.02081(15) Uani d 1 . . H H9A 0.147274 0.032787 0.665866 0.025 Uiso calc 1 . . H H9B 0.125732 -0.033851 0.569376 0.025 Uiso calc 1 . . C C10 0.25502(6) 0.08274(10) 0.59283(6) 0.02231(15) Uani d 1 . . C C11 0.32861(7) -0.02778(12) 0.63580(7) 0.0316(2) Uani d 1 . . H H11A 0.307193 -0.131044 0.619844 0.047 Uiso calc 1 . . H H11B 0.335063 -0.015875 0.699085 0.047 Uiso calc 1 . . H H11C 0.391777 -0.008787 0.616620 0.047 Uiso calc 1 . . C C12 0.10666(6) 0.47028(9) 0.39869(5) 0.01999(14) Uani d 1 . . H H12A 0.077300 0.570684 0.406183 0.024 Uiso calc 1 . . H H12B 0.063673 0.417265 0.351674 0.024 Uiso calc 1 . . C C13 0.20497(6) 0.49478(9) 0.36878(5) 0.01973(14) Uani d 1 . . C C14 0.37969(6) 0.45788(11) 0.39438(6) 0.02663(18) Uani d 1 . . C C15 0.42552(8) 0.33352(14) 0.36257(7) 0.0365(2) Uani d 1 . . C C16 0.51776(9) 0.3568(2) 0.33836(10) 0.0557(4) Uani d 1 . . H H16 0.550264 0.275060 0.315182 0.067 Uiso calc 1 . . C C17 0.56220(9) 0.4971(2) 0.34769(11) 0.0664(5) Uani d 1 . . H H17 0.625396 0.510315 0.332070 0.080 Uiso calc 1 . . C C18 0.51564(10) 0.6172(2) 0.37936(10) 0.0579(4) Uani d 1 . . H H18 0.547197 0.712839 0.385442 0.069 Uiso calc 1 . . C C19 0.42263(8) 0.60162(14) 0.40288(7) 0.0381(2) Uani d 1 . . C C20 0.37803(12) 0.18097(16) 0.35535(11) 0.0515(3) Uani d 1 . . H H20A 0.315758 0.187197 0.316412 0.077 Uiso calc 1 . . H H20B 0.366401 0.147447 0.413048 0.077 Uiso calc 1 . . H H20C 0.420847 0.108401 0.331858 0.077 Uiso calc 1 . . C C21 0.37171(12) 0.73438(15) 0.43604(10) 0.0528(3) Uani d 1 . . H H21A 0.322214 0.772932 0.389673 0.079 Uiso calc 1 . . H H21B 0.419331 0.814269 0.454501 0.079 Uiso calc 1 . . H H21C 0.340299 0.702735 0.485625 0.079 Uiso calc 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 O1 0.0214(3) 0.0181(3) 0.0320(3) -0.0025(2) 0.0089(2) 0.0019(2) O2 0.0324(3) 0.0196(3) 0.0212(3) -0.0036(2) 0.0045(2) -0.0041(2) O3 0.0261(3) 0.0303(3) 0.0419(4) -0.0001(3) 0.0079(3) 0.0139(3) O4 0.0303(3) 0.0361(4) 0.0206(3) 0.0004(3) 0.0053(2) 0.0107(2) N1 0.0230(3) 0.0147(3) 0.0162(3) -0.0012(2) 0.0045(2) 0.0007(2) N2 0.0221(3) 0.0242(3) 0.0213(3) 0.0006(2) 0.0051(2) 0.0069(2) C1 0.0214(3) 0.0153(3) 0.0178(3) -0.0010(2) 0.0045(2) -0.0007(2) C2 0.0296(4) 0.0157(3) 0.0237(3) -0.0032(3) 0.0062(3) -0.0013(3) C3 0.0348(4) 0.0198(4) 0.0266(4) -0.0037(3) 0.0057(3) -0.0062(3) C4 0.0356(5) 0.0269(4) 0.0203(3) -0.0020(3) 0.0044(3) -0.0053(3) C5 0.0311(4) 0.0226(4) 0.0179(3) -0.0012(3) 0.0049(3) 0.0008(3) C6 0.0226(3) 0.0153(3) 0.0179(3) -0.0010(2) 0.0044(2) -0.0002(2) C7 0.0206(3) 0.0145(3) 0.0193(3) -0.0019(2) 0.0050(2) 0.0012(2) C8 0.0196(3) 0.0155(3) 0.0193(3) -0.0005(2) 0.0037(2) -0.0005(2) C9 0.0235(3) 0.0157(3) 0.0236(3) 0.0004(3) 0.0045(3) 0.0029(3) C10 0.0236(3) 0.0200(3) 0.0236(3) 0.0015(3) 0.0044(3) 0.0010(3) C11 0.0271(4) 0.0310(4) 0.0374(5) 0.0081(3) 0.0072(3) 0.0093(4) C12 0.0228(3) 0.0196(3) 0.0180(3) 0.0010(3) 0.0043(3) 0.0041(2) C13 0.0237(3) 0.0186(3) 0.0173(3) -0.0003(3) 0.0044(3) 0.0011(2) C14 0.0215(3) 0.0354(5) 0.0230(4) -0.0008(3) 0.0034(3) 0.0095(3) C15 0.0299(4) 0.0478(6) 0.0334(5) 0.0128(4) 0.0102(4) 0.0136(4) C16 0.0342(5) 0.0853(11) 0.0517(7) 0.0270(6) 0.0199(5) 0.0313(7) C17 0.0237(5) 0.1103(14) 0.0668(9) 0.0030(7) 0.0118(5) 0.0503(10) C18 0.0323(5) 0.0797(10) 0.0591(8) -0.0212(6) -0.0020(5) 0.0332(8) C19 0.0328(5) 0.0454(6) 0.0342(5) -0.0131(4) -0.0010(4) 0.0135(4) C20 0.0586(8) 0.0398(6) 0.0598(8) 0.0159(6) 0.0215(7) -0.0014(6) C21 0.0691(9) 0.0350(6) 0.0522(7) -0.0196(6) 0.0019(6) -0.0015(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 O1 H1 . . 106.6(10) ? C8 N1 C1 . . 110.76(6) ? C8 N1 C12 . . 123.77(7) ? C1 N1 C12 . . 125.35(6) ? C13 N2 C14 . . 120.85(7) ? C13 N2 H2A . . 120.0(9) ? C14 N2 H2A . . 118.0(9) ? C2 C1 C6 . . 122.48(7) ? C2 C1 N1 . . 127.85(7) ? C6 C1 N1 . . 109.65(6) ? C1 C2 C3 . . 116.96(8) ? C1 C2 H2 . . 121.5 ? C3 C2 H2 . . 121.5 ? C4 C3 C2 . . 121.27(8) ? C4 C3 H3 . . 119.4 ? C2 C3 H3 . . 119.4 ? C3 C4 C5 . . 120.58(8) ? C3 C4 H4 . . 119.7 ? C5 C4 H4 . . 119.7 ? C6 C5 C4 . . 118.55(8) ? C6 C5 H5 . . 120.7 ? C4 C5 H5 . . 120.7 ? C5 C6 C1 . . 120.16(7) ? C5 C6 C7 . . 130.47(7) ? C1 C6 C7 . . 109.27(7) ? O1 C7 C6 . . 109.46(6) ? O1 C7 C9 . . 110.96(6) ? C6 C7 C9 . . 114.71(7) ? O1 C7 C8 . . 107.99(6) ? C6 C7 C8 . . 101.59(6) ? C9 C7 C8 . . 111.59(6) ? O2 C8 N1 . . 125.24(7) ? O2 C8 C7 . . 126.03(7) ? N1 C8 C7 . . 108.66(6) ? C10 C9 C7 . . 114.46(6) ? C10 C9 H9A . . 108.6 ? C7 C9 H9A . . 108.6 ? C10 C9 H9B . . 108.6 ? C7 C9 H9B . . 108.6 ? H9A C9 H9B . . 107.6 ? O3 C10 C11 . . 121.37(8) ? O3 C10 C9 . . 121.73(8) ? C11 C10 C9 . . 116.90(7) ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? N1 C12 C13 . . 116.66(7) ? N1 C12 H12A . . 108.1 ? C13 C12 H12A . . 108.1 ? N1 C12 H12B . . 108.1 ? C13 C12 H12B . . 108.1 ? H12A C12 H12B . . 107.3 ? O4 C13 N2 . . 123.73(8) ? O4 C13 C12 . . 118.34(7) ? N2 C13 C12 . . 117.91(7) ? C15 C14 C19 . . 122.55(10) ? C15 C14 N2 . . 118.49(9) ? C19 C14 N2 . . 118.96(9) ? C14 C15 C16 . . 117.43(13) ? C14 C15 C20 . . 121.16(10) ? C16 C15 C20 . . 121.41(12) ? C17 C16 C15 . . 120.95(14) ? C17 C16 H16 . . 119.5 ? C15 C16 H16 . . 119.5 ? C18 C17 C16 . . 120.38(11) ? C18 C17 H17 . . 119.8 ? C16 C17 H17 . . 119.8 ? C17 C18 C19 . . 121.27(14) ? C17 C18 H18 . . 119.4 ? C19 C18 H18 . . 119.4 ? C18 C19 C14 . . 117.39(13) ? C18 C19 C21 . . 120.81(13) ? C14 C19 C21 . . 121.80(10) ? C15 C20 H20A . . 109.5 ? C15 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C15 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? C19 C21 H21A . . 109.5 ? C19 C21 H21B . . 109.5 ? H21A C21 H21B . . 109.5 ? C19 C21 H21C . . 109.5 ? H21A C21 H21C . . 109.5 ? H21B C21 H21C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C7 . 1.4242(10) ? O1 H1 . 0.864(15) ? O2 C8 . 1.2248(9) ? O3 C10 . 1.2167(11) ? O4 C13 . 1.2266(10) ? N1 C8 . 1.3655(10) ? N1 C1 . 1.4170(10) ? N1 C12 . 1.4450(10) ? N2 C13 . 1.3467(11) ? N2 C14 . 1.4329(11) ? N2 H2A . 0.874(15) ? C1 C2 . 1.3840(11) ? C1 C6 . 1.3948(11) ? C2 C3 . 1.4026(12) ? C2 H2 . 0.9500 ? C3 C4 . 1.3913(13) ? C3 H3 . 0.9500 ? C4 C5 . 1.4017(13) ? C4 H4 . 0.9500 ? C5 C6 . 1.3818(11) ? C5 H5 . 0.9500 ? C6 C7 . 1.5087(11) ? C7 C9 . 1.5279(11) ? C7 C8 . 1.5501(11) ? C9 C10 . 1.5091(12) ? C9 H9A . 0.9900 ? C9 H9B . 0.9900 ? C10 C11 . 1.4965(13) ? C11 H11A . 0.9800 ? C11 H11B . 0.9800 ? C11 H11C . 0.9800 ? C12 C13 . 1.5187(11) ? C12 H12A . 0.9900 ? C12 H12B . 0.9900 ? C14 C15 . 1.3956(15) ? C14 C19 . 1.4005(15) ? C15 C16 . 1.4002(16) ? C15 C20 . 1.497(2) ? C16 C17 . 1.382(3) ? C16 H16 . 0.9500 ? C17 C18 . 1.370(3) ? C17 H17 . 0.9500 ? C18 C19 . 1.3976(17) ? C18 H18 . 0.9500 ? C19 C21 . 1.499(2) ? C20 H20A . 0.9800 ? C20 H20B . 0.9800 ? C20 H20C . 0.9800 ? C21 H21A . 0.9800 ? C21 H21B . 0.9800 ? C21 H21C . 0.9800 ? 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 O1 H1 O2 3_556 0.864(15) 1.942(15) 2.7829(9) 164.1(14) yes N2 H2A O3 . 0.874(15) 2.154(15) 3.0193(10) 170.3(13) yes C3 H3 O4 4_576 0.95 2.44 3.3280(12) 155 y C9 H9A O4 4_566 0.99 2.33 3.2537(11) 154 yes C11 H11B O4 4_566 0.98 2.59 3.2988(12) 129 yes C12 H12A O1 3_566 0.99 2.60 3.5835(11) 173 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 C8 N1 C1 C2 . . . . -178.96(8) ? C12 N1 C1 C2 . . . . -2.79(13) ? C8 N1 C1 C6 . . . . -0.65(9) ? C12 N1 C1 C6 . . . . 175.53(7) ? C6 C1 C2 C3 . . . . -0.55(13) ? N1 C1 C2 C3 . . . . 177.57(8) ? C1 C2 C3 C4 . . . . 0.25(14) ? C2 C3 C4 C5 . . . . -0.08(15) ? C3 C4 C5 C6 . . . . 0.18(14) ? C4 C5 C6 C1 . . . . -0.47(13) ? C4 C5 C6 C7 . . . . -176.29(8) ? C2 C1 C6 C5 . . . . 0.68(13) ? N1 C1 C6 C5 . . . . -177.74(7) ? C2 C1 C6 C7 . . . . 177.32(7) ? N1 C1 C6 C7 . . . . -1.11(9) ? C5 C6 C7 O1 . . . . 64.33(11) ? C1 C6 C7 O1 . . . . -111.85(7) ? C5 C6 C7 C9 . . . . -61.13(12) ? C1 C6 C7 C9 . . . . 122.69(7) ? C5 C6 C7 C8 . . . . 178.34(9) ? C1 C6 C7 C8 . . . . 2.16(8) ? C1 N1 C8 O2 . . . . 179.22(8) ? C12 N1 C8 O2 . . . . 2.97(12) ? C1 N1 C8 C7 . . . . 2.07(9) ? C12 N1 C8 C7 . . . . -174.18(7) ? O1 C7 C8 O2 . . . . -64.57(10) ? C6 C7 C8 O2 . . . . -179.67(8) ? C9 C7 C8 O2 . . . . 57.64(10) ? O1 C7 C8 N1 . . . . 112.55(7) ? C6 C7 C8 N1 . . . . -2.55(8) ? C9 C7 C8 N1 . . . . -125.24(7) ? O1 C7 C9 C10 . . . . 177.23(7) ? C6 C7 C9 C10 . . . . -58.09(9) ? C8 C7 C9 C10 . . . . 56.75(9) ? C7 C9 C10 O3 . . . . -13.37(12) ? C7 C9 C10 C11 . . . . 167.08(8) ? C8 N1 C12 C13 . . . . -98.64(9) ? C1 N1 C12 C13 . . . . 85.66(9) ? C14 N2 C13 O4 . . . . -0.69(13) ? C14 N2 C13 C12 . . . . -179.30(8) ? N1 C12 C13 O4 . . . . -179.12(8) ? N1 C12 C13 N2 . . . . -0.44(11) ? C13 N2 C14 C15 . . . . -107.45(10) ? C13 N2 C14 C19 . . . . 71.84(12) ? C19 C14 C15 C16 . . . . -0.29(15) ? N2 C14 C15 C16 . . . . 178.98(9) ? C19 C14 C15 C20 . . . . 179.24(11) ? N2 C14 C15 C20 . . . . -1.49(15) ? C14 C15 C16 C17 . . . . 1.46(18) ? C20 C15 C16 C17 . . . . -178.06(13) ? C15 C16 C17 C18 . . . . -1.3(2) ? C16 C17 C18 C19 . . . . -0.1(2) ? C17 C18 C19 C14 . . . . 1.18(18) ? C17 C18 C19 C21 . . . . -178.97(13) ? C15 C14 C19 C18 . . . . -1.01(15) ? N2 C14 C19 C18 . . . . 179.73(10) ? C15 C14 C19 C21 . . . . 179.15(11) ? N2 C14 C19 C21 . . . . -0.12(15) ? _cod_database_fobs_code 2244147