#------------------------------------------------------------------------------ #$Date: 2023-08-16 04:47:53 +0300 (Wed, 16 Aug 2023) $ #$Revision: 285783 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/02/28/2022834.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_2022834 loop_ _publ_author_name 'Decato, Daniel' 'Jahnke, Michael' 'Berryman, Orion' _publ_section_title ; Conformational polymorphism of 3-(azidomethyl)benzoic acid ; _journal_coeditor_code EQ3010 _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C Structural Chemistry' _journal_paper_doi 10.1107/S2053229623006824 _journal_volume 79 _journal_year 2023 _chemical_formula_iupac 'C8 H7 N3 O2' _chemical_formula_moiety 'C8 H7 N3 O2' _chemical_formula_sum 'C8 H7 N3 O2' _chemical_formula_weight 177.17 _chemical_name_systematic ; 3-(Azidomethyl)benzoic acid ; _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 _audit_creation_method ;FinalCif V117 by Daniel Kratzert, Freiburg 2023, https://dkratzert.de/finalcif.html ; _cell_angle_alpha 90 _cell_angle_beta 104.095(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6327(5) _cell_length_b 9.5561(6) _cell_length_c 11.2899(7) _cell_measurement_reflns_used 7334 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.032 _cell_measurement_theta_min 2.752 _cell_volume 798.68(9) _computing_cell_refinement ; SAINT (Bruker, 2016) ; _computing_data_collection ; APEX4 (Bruker, 2021) ; _computing_data_reduction ; SAINT (Bruker, 2016) ; _computing_molecular_graphics ; OLEX2 (Dolomanov et al., 2009) ; _computing_publication_material ; OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker Photon II' _diffrn_detector_area_resol_mean 7.39 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'Fixed Chi Three-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE DUO' _diffrn_measurement_method '\w and \f scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_radiation_monochromator 'TRIUMPH graphite' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_unetI/netI 0.0294 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 21950 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.408 _diffrn_reflns_theta_min 2.751 _diffrn_source 'sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.473 _exptl_crystal_description plate _exptl_crystal_F_000 368 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.322 _refine_diff_density_min -0.227 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 122 _refine_ls_number_reflns 1988 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0408 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.4603P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.1006 _reflns_number_gt 1496 _reflns_number_total 1988 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file eq3010sup1.cif _cod_data_source_block A _cod_database_code 2022834 _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 0.983 _shelx_estimated_absorpt_t_max 0.996 _shelx_hkl_file ; -1 0 0 123.09 5.10 1 0 0 115.39 5.20 1 0 0 109.09 4.90 1 0 0 122.09 5.20 -1 0 0 121.39 4.50 -2 0 0 853.51 29.10 -2 0 0 853.31 29.20 -2 0 0 805.72 29.10 -2 0 0 849.02 29.40 2 0 0 850.11 28.60 2 0 0 845.42 29.00 2 0 0 883.81 29.40 2 0 0 859.71 29.30 2 0 0 864.61 28.50 2 0 0 849.12 29.20 3 0 0 1368.96 49.70 -3 0 0 1420.46 49.60 3 0 0 1448.06 49.20 3 0 0 1521.75 49.00 3 0 0 1430.16 49.40 3 0 0 1495.35 49.60 3 0 0 1509.35 49.90 3 0 0 1465.55 49.40 -3 0 0 1482.35 49.80 -3 0 0 1477.45 49.50 -3 0 0 1520.45 50.29 -3 0 0 1486.75 48.90 -4 0 0 660.63 25.10 4 0 0 663.63 24.80 4 0 0 668.33 24.50 4 0 0 678.93 25.20 4 0 0 705.23 23.90 4 0 0 694.33 23.70 4 0 0 679.23 25.50 -4 0 0 641.94 23.60 4 0 0 655.03 24.50 -4 0 0 665.63 24.70 -4 0 0 663.93 25.00 4 0 0 665.13 23.50 5 0 0 211.98 9.90 5 0 0 218.18 12.80 5 0 0 199.58 9.70 5 0 0 206.98 10.80 5 0 0 204.18 12.20 5 0 0 197.58 11.20 -5 0 0 223.38 11.80 -5 0 0 199.38 9.60 -5 0 0 199.08 12.20 5 0 0 205.88 11.00 -5 0 0 213.78 12.50 5 0 0 199.08 9.30 6 0 0 471.65 19.00 -6 0 0 513.45 21.70 -6 0 0 469.15 21.10 6 0 0 425.86 19.60 -6 0 0 493.65 21.10 6 0 0 499.45 19.10 6 0 0 476.75 18.50 6 0 0 493.45 22.10 -6 0 0 456.35 18.90 6 0 0 481.05 21.30 7 0 0 -2.30 4.10 -7 0 0 -2.20 8.10 7 0 0 3.90 4.30 7 0 0 -8.80 8.30 7 0 0 -0.50 9.20 -7 0 0 7.60 7.40 -7 0 0 -3.30 7.60 -8 0 0 25.00 9.70 -8 0 0 15.20 9.30 8 0 0 29.80 11.70 8 0 0 19.20 6.40 8 0 0 15.60 10.70 8 0 0 31.20 6.40 -8 0 0 28.00 10.60 9 0 0 -1.30 5.50 9 0 0 -10.30 12.30 9 0 0 -7.10 12.20 9 0 0 2.70 5.30 -9 0 0 -5.60 9.50 -9 0 0 -11.90 9.80 -9 0 0 1.10 9.70 1 -1 0 235.98 8.70 -1 -1 0 238.48 9.90 1 -1 0 239.58 9.40 1 -1 0 261.97 9.60 1 -1 0 249.48 9.10 -1 -1 0 237.58 9.30 -1 -1 0 254.97 8.60 -1 -1 0 246.78 9.00 1 -1 0 259.57 8.30 1 -1 0 245.18 9.20 -1 1 0 245.28 8.90 -1 1 0 250.57 9.30 1 1 0 256.57 8.90 1 1 0 250.07 8.90 1 1 0 253.27 9.60 1 1 0 229.08 9.20 -1 1 0 242.58 8.30 1 1 0 242.98 8.70 -1 1 0 242.68 9.90 -1 1 0 245.88 8.80 -1 1 0 242.48 9.50 1 1 0 244.98 9.20 2 -1 0 5863.81 188.48 2 -1 0 5517.65 188.88 2 -1 0 6290.87 189.28 2 -1 0 5796.92 188.78 -2 -1 0 5913.51 188.28 -2 -1 0 6050.59 188.98 2 -1 0 5784.22 188.78 -2 -1 0 5718.63 188.48 -2 -1 0 5832.42 189.08 -2 -1 0 5319.67 188.78 2 1 0 5529.15 188.88 2 1 0 5808.62 188.98 2 1 0 5828.62 188.48 2 1 0 5745.73 188.88 -2 1 0 5945.21 188.48 -2 1 0 5951.70 188.98 -2 1 0 5832.62 188.98 3 -1 0 475.65 18.80 -3 -1 0 519.25 18.60 -3 -1 0 523.95 17.80 3 -1 0 515.85 17.60 3 -1 0 494.45 19.00 -3 -1 0 445.66 18.50 -3 -1 0 517.95 19.40 -3 -1 0 510.35 19.60 3 -1 0 537.35 19.30 3 -1 0 511.55 18.50 3 -1 0 519.25 18.30 3 -1 0 531.55 19.50 3 1 0 503.15 19.30 -3 1 0 466.95 19.10 3 1 0 521.75 19.30 3 1 0 498.95 19.00 3 1 0 493.45 18.40 -3 1 0 500.45 18.50 -3 1 0 505.05 18.10 3 1 0 502.95 19.10 3 1 0 504.35 18.00 -3 1 0 505.15 19.30 -4 -1 0 76.69 9.30 -4 -1 0 93.09 8.50 -4 -1 0 88.29 6.00 4 -1 0 90.19 6.40 4 -1 0 88.29 5.50 4 -1 0 81.99 8.00 4 -1 0 92.59 6.90 4 -1 0 69.59 8.00 4 -1 0 92.39 7.70 4 -1 0 72.69 9.30 -4 -1 0 88.89 8.00 -4 1 0 98.49 7.70 -4 1 0 86.69 9.00 4 1 0 91.49 6.40 4 1 0 78.79 7.90 4 1 0 84.79 7.80 -4 1 0 96.89 5.80 4 1 0 93.49 6.40 4 1 0 82.49 7.80 -4 1 0 98.79 8.30 4 1 0 95.09 8.10 4 1 0 83.39 9.10 4 1 0 94.19 5.60 5 -1 0 132.89 7.20 -5 -1 0 136.29 10.70 -5 -1 0 123.89 9.70 5 -1 0 133.79 8.00 5 -1 0 131.39 8.70 -5 -1 0 114.29 7.00 5 -1 0 130.79 6.80 5 -1 0 118.79 8.90 -5 -1 0 132.39 10.60 5 -1 0 128.99 10.10 -5 1 0 129.69 10.70 -5 1 0 117.09 10.60 5 1 0 125.89 7.90 5 1 0 147.99 9.60 -5 1 0 129.89 9.70 5 1 0 130.99 7.60 5 1 0 139.49 11.30 5 1 0 111.69 9.10 5 1 0 124.79 9.10 5 1 0 121.99 9.90 6 -1 0 148.99 9.10 6 -1 0 172.88 9.20 6 -1 0 149.29 10.60 -6 -1 0 168.28 9.00 -6 -1 0 168.18 11.90 6 -1 0 146.39 13.20 6 -1 0 164.78 12.60 6 -1 0 162.08 10.10 -6 -1 0 167.68 12.00 -6 -1 0 181.28 13.80 6 1 0 153.08 13.60 6 1 0 160.58 10.10 6 1 0 180.28 12.50 -6 1 0 168.48 11.80 -6 1 0 181.18 12.90 6 1 0 177.28 14.00 -6 1 0 182.38 12.80 6 1 0 175.78 9.50 6 1 0 175.58 10.10 -7 -1 0 -0.80 7.60 -7 -1 0 -1.70 6.80 7 -1 0 9.90 9.00 7 -1 0 11.10 5.50 -7 -1 0 7.40 8.10 7 -1 0 1.70 7.90 7 -1 0 -8.10 4.00 7 1 0 2.50 4.70 7 1 0 4.20 4.90 7 1 0 0.70 9.40 -7 1 0 -11.00 7.80 7 1 0 6.60 8.90 -7 1 0 20.70 8.60 -7 1 0 -6.00 7.80 8 -1 0 38.70 11.80 -8 -1 0 52.89 10.20 8 -1 0 56.09 6.60 8 -1 0 38.70 6.60 -8 -1 0 37.10 10.90 -8 -1 0 53.49 9.80 8 1 0 47.00 12.60 -8 1 0 46.60 9.50 -8 1 0 61.69 11.10 8 1 0 60.39 7.30 8 1 0 38.20 11.10 -8 1 0 58.69 10.40 9 -1 0 35.10 12.10 -9 -1 0 33.20 10.60 9 -1 0 15.50 12.50 9 -1 0 34.10 6.60 -9 -1 0 29.80 10.60 9 1 0 15.80 13.50 9 1 0 9.70 11.90 -9 1 0 33.70 10.20 9 1 0 34.50 6.30 9 1 0 49.00 8.30 -9 1 0 45.00 11.00 -9 1 0 49.40 12.00 0 -2 0 1795.82 58.59 0 -2 0 1595.34 58.99 0 -2 0 1814.12 58.69 0 2 0 1869.41 58.79 0 2 0 1870.31 58.59 0 2 0 1656.03 58.59 0 2 0 1843.02 58.89 0 2 0 1812.12 58.69 0 2 0 1855.41 58.39 -1 -2 0 1017.30 37.70 -1 -2 0 1156.78 37.70 1 -2 0 1021.30 37.80 -1 -2 0 1094.59 37.60 1 -2 0 1142.79 36.90 1 -2 0 1172.08 38.40 -1 -2 0 1160.68 37.70 1 -2 0 1115.69 37.70 -1 -2 0 1134.59 38.30 -1 2 0 1119.89 38.30 -1 2 0 1174.38 37.90 1 2 0 1162.78 37.60 -1 2 0 1175.68 36.90 1 2 0 1152.48 38.20 1 2 0 1140.09 37.60 -1 2 0 1118.29 37.60 -1 2 0 1189.58 38.00 1 2 0 1154.18 37.80 1 2 0 1094.89 38.20 1 2 0 1143.99 37.30 -2 -2 0 2.80 3.80 2 -2 0 10.10 3.20 -2 -2 0 6.10 5.10 2 -2 0 6.40 1.50 -2 -2 0 4.40 3.10 2 -2 0 7.10 3.50 2 -2 0 5.60 2.50 2 -2 0 13.10 4.50 2 -2 0 14.00 4.70 -2 2 0 10.10 2.90 2 2 0 7.00 4.50 2 2 0 7.50 4.40 2 2 0 8.90 2.80 -2 2 0 6.90 4.90 2 2 0 5.10 3.40 -2 2 0 9.20 4.10 2 2 0 5.20 2.00 2 2 0 2.70 2.90 -2 2 0 4.90 1.50 -2 2 0 11.20 4.40 -2 2 0 5.60 3.10 3 -2 0 5.50 4.80 3 -2 0 3.30 4.90 3 -2 0 1.90 2.00 -3 -2 0 2.10 2.40 -3 -2 0 3.00 3.40 -3 -2 0 5.90 5.40 -3 -2 0 -2.10 4.20 3 -2 0 1.40 4.50 3 -2 0 -2.20 3.90 3 -2 0 4.10 2.80 3 -2 0 1.30 3.10 3 2 0 -2.20 3.00 3 2 0 4.40 3.60 3 2 0 0.80 4.90 -3 2 0 12.40 5.40 3 2 0 2.70 4.00 3 2 0 2.90 5.10 -3 2 0 5.30 5.00 -3 2 0 11.90 4.60 -3 2 0 3.10 3.70 -3 2 0 1.80 2.60 3 2 0 2.00 3.00 3 2 0 2.40 3.90 -4 -2 0 526.25 20.60 4 -2 0 547.65 19.60 -4 -2 0 526.95 19.40 4 -2 0 511.45 19.10 -4 -2 0 517.25 18.50 4 -2 0 491.75 20.00 4 -2 0 482.55 21.40 4 -2 0 480.35 20.80 4 -2 0 488.35 20.00 -4 -2 0 507.65 21.10 4 2 0 494.85 20.30 -4 2 0 510.25 19.00 4 2 0 513.05 19.10 4 2 0 533.15 20.60 -4 2 0 509.25 20.70 4 2 0 543.55 18.80 4 2 0 537.45 19.70 -4 2 0 522.55 20.50 4 2 0 518.85 20.20 -4 2 0 532.95 19.20 5 -2 0 69.79 8.90 5 -2 0 83.39 7.30 5 -2 0 85.59 7.40 -5 -2 0 91.79 6.00 5 -2 0 84.69 9.50 5 -2 0 72.89 8.70 -5 -2 0 92.39 8.10 5 -2 0 76.79 7.90 5 -2 0 86.29 5.70 -5 -2 0 97.69 10.60 -5 -2 0 88.99 9.70 5 2 0 90.59 8.50 -5 2 0 70.99 6.10 5 2 0 102.29 9.50 5 2 0 85.19 6.90 5 2 0 84.99 6.50 5 2 0 83.49 6.90 5 2 0 81.99 9.20 5 2 0 70.19 8.40 -5 2 0 82.79 9.50 -5 2 0 76.69 10.20 -5 2 0 73.19 8.10 5 2 0 66.49 8.60 -6 -2 0 1.20 6.60 -6 -2 0 -3.30 7.60 6 -2 0 3.40 7.60 6 -2 0 6.00 7.40 6 -2 0 2.50 3.10 6 -2 0 0.90 4.40 -6 -2 0 -1.00 3.50 -6 -2 0 0.00 5.40 6 -2 0 -7.30 4.50 6 -2 0 5.90 3.20 6 2 0 1.00 4.10 6 2 0 0.10 4.40 -6 2 0 12.20 8.50 -6 2 0 6.30 6.20 6 2 0 -10.30 7.30 6 2 0 13.90 7.10 -6 2 0 -4.00 7.60 6 2 0 -11.00 7.10 -7 -2 0 5.20 7.80 7 -2 0 16.10 9.20 7 -2 0 0.50 8.60 -7 -2 0 -4.20 6.50 7 -2 0 3.10 3.70 7 -2 0 3.30 5.70 -7 2 0 9.10 8.70 -7 2 0 4.20 6.60 7 2 0 0.60 9.90 -7 2 0 3.70 8.40 7 2 0 -1.70 4.00 7 2 0 -2.00 9.80 8 -2 0 -7.10 9.30 -8 -2 0 6.20 11.20 8 -2 0 12.60 4.60 8 -2 0 7.40 10.20 8 -2 0 5.30 5.60 -8 -2 0 0.40 8.70 -8 -2 0 -0.40 8.50 8 2 0 4.20 11.80 8 2 0 6.70 6.10 8 2 0 11.90 4.80 -8 2 0 8.50 10.60 8 2 0 7.10 10.10 -8 2 0 0.90 9.00 -8 2 0 3.80 8.10 -9 -2 0 24.50 10.40 9 -2 0 10.40 6.20 -9 -2 0 9.20 10.90 9 -2 0 -1.40 11.10 9 -2 0 10.50 12.40 -9 2 0 20.90 10.50 9 2 0 15.30 6.90 9 2 0 21.00 12.00 9 2 0 23.50 6.20 -9 2 0 1.40 9.40 -9 2 0 25.70 12.50 9 2 0 9.90 14.10 0 -3 0 -1.10 2.10 0 -3 0 -0.90 2.10 0 -3 0 -0.60 3.80 0 -3 0 2.70 4.00 0 3 0 2.20 4.00 0 3 0 -2.20 3.30 0 3 0 -1.20 2.30 0 3 0 1.20 2.60 1 -3 0 66.99 5.50 1 -3 0 59.89 3.30 -1 -3 0 62.99 6.90 -1 -3 0 52.79 5.30 -1 -3 0 65.39 4.60 -1 -3 0 50.79 5.40 -1 -3 0 68.99 5.90 1 -3 0 53.99 4.90 1 -3 0 56.89 5.80 1 -3 0 63.79 6.20 -1 -3 0 53.79 4.90 -1 3 0 54.19 5.90 -1 3 0 59.89 3.10 1 3 0 56.89 5.00 1 3 0 55.19 4.20 -1 3 0 51.99 5.00 1 3 0 54.09 6.10 -1 3 0 61.09 6.30 1 3 0 45.60 5.10 -1 3 0 50.49 4.50 -1 3 0 60.19 4.70 1 3 0 51.09 5.10 1 3 0 59.89 4.10 2 -3 0 2155.68 70.59 -2 -3 0 2168.48 71.39 2 -3 0 2143.89 70.89 2 -3 0 1969.50 71.19 2 -3 0 2151.58 69.19 -2 -3 0 2181.68 70.29 2 -3 0 2089.09 70.59 -2 -3 0 2047.60 70.69 2 3 0 2222.98 69.99 -2 3 0 2137.69 71.19 2 3 0 2169.58 70.79 2 3 0 2129.29 70.49 -2 3 0 2033.50 69.69 -2 3 0 2212.88 69.29 -2 3 0 2214.48 70.89 2 3 0 2130.89 70.19 2 3 0 2115.89 71.19 -2 3 0 2124.09 70.49 2 3 0 2070.09 70.59 3 -3 0 203.58 7.50 -3 -3 0 210.58 12.20 3 -3 0 180.28 10.40 3 -3 0 197.58 9.90 -3 -3 0 203.68 10.50 3 -3 0 199.08 11.00 3 -3 0 201.98 9.30 -3 -3 0 212.98 8.40 3 -3 0 179.78 10.30 3 3 0 196.18 8.90 3 3 0 183.18 10.80 3 3 0 213.08 10.00 -3 3 0 207.18 8.90 -3 3 0 226.58 11.30 -3 3 0 197.38 9.20 -3 3 0 195.68 7.40 3 3 0 214.88 11.10 -3 3 0 201.88 11.70 3 3 0 207.88 8.60 3 3 0 197.88 9.10 4 -3 0 31.50 3.10 -4 -3 0 35.00 3.50 4 -3 0 28.80 6.00 4 -3 0 38.70 4.40 4 -3 0 39.50 7.10 -4 -3 0 43.70 7.40 4 -3 0 25.40 3.80 -4 -3 0 29.20 4.50 -4 -3 0 37.70 5.70 4 3 0 36.90 4.30 4 3 0 34.20 5.80 4 3 0 36.70 5.80 -4 3 0 32.90 4.50 -4 3 0 46.00 6.80 4 3 0 34.10 6.20 4 3 0 38.50 4.90 4 3 0 38.20 4.20 4 3 0 33.20 7.10 -4 3 0 38.10 7.50 -5 -3 0 84.89 9.60 5 -3 0 87.19 7.00 -5 -3 0 92.29 6.00 5 -3 0 92.79 9.90 5 -3 0 65.09 8.90 5 -3 0 84.09 8.00 -5 -3 0 85.99 11.50 5 -3 0 88.89 5.20 -5 -3 0 95.39 8.20 5 3 0 84.89 9.30 5 3 0 91.69 7.20 5 3 0 95.09 8.40 -5 3 0 102.59 11.10 -5 3 0 94.29 8.10 5 3 0 84.99 11.00 -5 3 0 92.79 10.40 -5 3 0 80.29 7.10 5 3 0 82.99 9.00 -6 -3 0 313.87 17.10 6 -3 0 304.17 12.10 -6 -3 0 304.07 14.70 6 -3 0 335.77 18.20 6 -3 0 352.36 15.40 -6 -3 0 308.77 18.50 6 -3 0 298.47 14.30 6 3 0 307.97 15.40 6 3 0 324.87 14.10 -6 3 0 312.77 17.90 6 3 0 275.97 16.80 6 3 0 333.97 18.40 -6 3 0 320.07 14.70 -6 3 0 301.67 19.00 6 3 0 302.37 14.90 -7 -3 0 12.30 9.70 7 -3 0 15.40 9.10 -7 -3 0 7.90 8.20 7 -3 0 -1.40 8.70 7 -3 0 19.40 5.90 -7 -3 0 1.20 6.70 7 -3 0 -1.20 3.60 -7 3 0 6.60 10.80 7 3 0 6.70 5.20 7 3 0 8.10 4.70 7 3 0 2.60 9.30 -7 3 0 3.50 9.00 7 3 0 2.10 10.90 -7 3 0 0.90 6.20 -8 -3 0 40.40 12.50 8 -3 0 49.40 7.50 8 -3 0 29.20 12.20 8 -3 0 36.40 11.40 -8 -3 0 44.60 10.00 -8 -3 0 40.80 8.90 8 3 0 48.80 6.40 8 3 0 59.09 7.50 -8 3 0 52.19 10.90 8 3 0 52.49 12.60 -8 3 0 69.29 13.10 -8 3 0 53.19 8.50 -9 -3 0 23.00 13.00 9 -3 0 12.60 12.00 9 -3 0 -4.70 12.10 9 -3 0 28.70 7.00 -9 -3 0 -5.40 9.40 -9 3 0 12.20 10.70 9 3 0 40.00 14.90 9 3 0 27.70 5.90 -9 3 0 22.50 12.10 9 3 0 16.50 11.40 9 3 0 31.80 7.90 0 -4 0 4218.38 140.59 0 4 0 4215.68 140.49 0 4 0 4261.37 140.99 0 4 0 4351.46 140.69 0 4 0 4433.26 141.39 0 4 0 4287.17 140.19 0 4 0 4385.76 140.79 1 -4 0 1135.29 37.10 -1 -4 0 1115.49 38.20 -1 -4 0 1126.89 37.80 -1 -4 0 1165.38 38.30 -1 -4 0 1121.69 38.20 -1 -4 0 1136.99 38.70 1 -4 0 1154.18 38.10 -1 -4 0 998.80 38.00 1 4 0 1112.39 37.80 1 4 0 1155.88 38.10 -1 4 0 1034.20 38.00 -1 4 0 1146.09 37.40 1 4 0 1045.30 38.10 1 4 0 1132.69 38.10 -1 4 0 1109.39 37.90 1 4 0 1140.79 38.50 -1 4 0 1136.39 38.20 1 4 0 1170.68 37.70 -2 -4 0 24.20 4.20 2 -4 0 18.80 2.30 -2 -4 0 24.10 6.00 -2 -4 0 21.00 4.60 2 -4 0 26.10 5.60 2 -4 0 29.20 5.20 2 -4 0 22.90 3.90 -2 -4 0 32.60 4.70 2 -4 0 20.80 3.50 -2 4 0 25.90 6.20 -2 4 0 23.10 3.10 2 4 0 23.30 3.00 2 4 0 27.90 3.70 -2 4 0 19.30 2.20 -2 4 0 23.60 4.70 2 4 0 19.20 4.20 2 4 0 20.20 2.70 -2 4 0 20.70 4.50 2 4 0 18.00 3.80 2 4 0 18.70 5.00 -2 4 0 26.80 3.70 3 -4 0 45.20 2.60 3 -4 0 42.20 6.00 -3 -4 0 46.50 6.40 -3 -4 0 63.29 7.50 -3 -4 0 44.30 5.30 3 -4 0 47.10 6.60 3 -4 0 37.30 4.70 3 -4 0 48.00 5.60 3 4 0 32.90 4.80 3 4 0 28.40 6.30 3 4 0 48.70 5.10 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-4 0 19.00 6.80 -7 -4 0 7.00 8.00 7 4 0 18.50 11.30 7 4 0 17.50 5.00 7 4 0 12.50 12.00 -7 4 0 18.30 10.80 -7 4 0 13.40 6.20 7 4 0 18.80 6.70 -7 4 0 9.50 9.60 8 -4 0 59.79 7.90 -8 -4 0 61.89 12.10 8 -4 0 33.90 13.10 -8 -4 0 66.39 10.90 8 4 0 56.19 6.80 -8 4 0 65.79 11.70 8 4 0 54.29 12.10 8 4 0 54.39 8.60 8 4 0 42.00 16.10 -8 4 0 59.59 12.80 9 -4 0 27.60 12.30 9 -4 0 25.70 14.40 9 -4 0 8.50 6.70 -9 -4 0 -12.90 10.80 -9 -4 0 1.40 9.80 9 4 0 -3.00 11.00 -9 4 0 1.70 10.50 -9 4 0 -6.30 13.50 9 4 0 -4.90 13.80 9 4 0 -1.40 7.10 0 -5 0 3.60 4.30 0 -5 0 -0.10 4.00 0 -5 0 0.10 2.50 0 -5 0 -0.90 2.60 0 5 0 -1.70 3.00 0 5 0 0.30 2.50 0 5 0 -0.80 3.40 0 5 0 -2.00 4.20 0 5 0 -0.30 4.00 0 5 0 -0.90 2.30 -1 -5 0 636.74 23.00 -1 -5 0 663.73 23.10 1 -5 0 622.84 21.50 1 -5 0 556.84 22.60 -1 -5 0 651.23 23.90 1 -5 0 634.34 22.60 -1 -5 0 583.24 22.80 -1 -5 0 623.44 23.20 1 5 0 648.44 22.20 1 5 0 642.44 22.80 1 5 0 605.34 23.10 -1 5 0 630.04 23.10 1 5 0 626.54 22.30 1 5 0 612.94 22.80 -1 5 0 625.14 23.50 -1 5 0 650.83 22.30 -1 5 0 623.54 22.40 -1 5 0 636.94 21.50 2 -5 0 351.96 12.40 -2 -5 0 367.96 16.20 2 -5 0 322.47 15.70 -2 -5 0 357.26 14.80 -2 -5 0 361.66 14.80 2 -5 0 339.67 14.80 2 -5 0 356.06 14.20 -2 -5 0 354.26 14.40 2 5 0 359.86 13.50 2 5 0 373.06 14.70 -2 5 0 369.26 16.70 -2 5 0 362.16 12.40 2 5 0 325.47 13.90 -2 5 0 330.47 14.90 -2 5 0 325.57 14.80 2 5 0 377.56 13.70 2 5 0 360.56 14.10 2 5 0 346.37 15.20 3 -5 0 42.30 6.90 3 -5 0 35.30 4.50 -3 -5 0 36.10 5.40 -3 -5 0 38.00 5.30 -3 -5 0 50.29 7.60 3 -5 0 37.90 2.50 3 5 0 33.50 5.80 3 5 0 45.40 6.90 -3 5 0 38.80 4.70 -3 5 0 38.90 2.50 3 5 0 34.10 4.30 -3 5 0 32.40 8.10 3 5 0 37.60 4.40 3 5 0 34.00 4.10 -3 5 0 44.60 6.10 3 5 0 45.20 4.30 4 -5 0 53.49 6.60 -4 -5 0 61.79 8.80 -4 -5 0 59.59 7.70 4 -5 0 59.99 7.50 4 -5 0 50.29 6.50 4 -5 0 47.30 5.20 -4 -5 0 56.69 6.80 4 -5 0 48.30 7.50 -4 5 0 71.99 9.80 4 5 0 67.89 6.20 4 5 0 64.99 8.20 4 5 0 60.89 5.70 -4 5 0 57.99 9.50 4 5 0 50.59 8.20 -4 5 0 56.99 5.60 5 -5 0 71.99 8.80 5 -5 0 74.09 8.60 -5 -5 0 61.79 8.10 -5 -5 0 71.69 9.90 5 -5 0 59.39 6.10 -5 -5 0 72.89 9.40 5 -5 0 71.99 10.40 5 5 0 62.89 8.20 5 5 0 59.99 10.10 -5 5 0 72.09 10.10 -5 5 0 74.49 10.80 5 5 0 77.19 11.00 5 5 0 70.19 7.10 -5 5 0 55.09 6.30 6 -5 0 4.90 8.20 6 -5 0 -4.40 7.20 6 -5 0 -0.50 5.30 -6 -5 0 2.90 7.10 -6 -5 0 2.50 5.70 -6 -5 0 14.10 9.70 6 5 0 -0.90 8.40 -6 5 0 6.60 4.80 -6 5 0 -4.80 8.60 6 5 0 0.70 4.60 6 5 0 -3.90 10.20 6 5 0 8.40 5.40 -6 5 0 26.00 11.40 7 -5 0 -10.80 9.40 -7 -5 0 11.50 10.50 7 -5 0 -1.50 5.60 7 -5 0 6.60 9.10 -7 -5 0 5.90 6.50 -7 -5 0 2.00 8.10 7 5 0 -1.30 4.60 7 5 0 7.00 11.30 -7 5 0 9.60 12.70 7 5 0 0.70 6.50 7 5 0 0.60 12.20 -7 5 0 -8.60 10.30 8 -5 0 4.80 11.90 8 -5 0 4.40 6.40 -8 -5 0 7.10 9.10 -8 -5 0 10.80 11.40 8 -5 0 34.70 11.80 8 5 0 17.60 5.60 -8 5 0 15.30 14.00 8 5 0 14.50 7.50 -8 5 0 8.90 10.30 8 5 0 9.10 14.30 8 5 0 3.80 14.60 9 -5 0 2.70 6.60 -9 -5 0 5.40 10.40 9 -5 0 -7.30 10.90 9 -5 0 -14.10 11.80 -9 -5 0 31.50 12.60 -9 5 0 -4.70 13.20 9 5 0 -9.50 7.40 9 5 0 11.40 15.40 9 5 0 -10.60 11.00 -9 5 0 -13.60 10.30 0 -6 0 75.49 6.10 0 -6 0 66.09 6.70 0 6 0 77.69 5.50 0 6 0 75.79 7.00 0 6 0 76.19 4.90 0 6 0 78.59 5.80 0 6 0 79.49 6.90 -1 -6 0 5.40 4.70 1 -6 0 -3.30 2.30 1 -6 0 2.10 5.00 1 -6 0 2.70 2.90 1 -6 0 6.40 4.70 1 6 0 1.90 2.10 1 6 0 -4.80 2.70 1 6 0 -5.10 3.60 -1 6 0 0.50 3.20 -1 6 0 -0.40 3.80 -1 6 0 4.50 5.00 -1 6 0 -3.10 5.80 1 6 0 4.30 4.30 -1 6 0 -4.80 3.80 -1 6 0 1.50 2.50 -1 6 0 2.70 4.00 1 6 0 -0.20 2.30 -2 -6 0 20.20 5.10 -2 -6 0 16.00 6.30 -2 -6 0 22.80 6.00 2 -6 0 17.40 6.20 2 -6 0 24.20 2.90 -2 -6 0 23.40 5.20 2 -6 0 23.00 4.00 2 6 0 23.10 4.50 2 6 0 19.60 5.00 -2 6 0 22.20 4.00 2 6 0 23.90 3.40 2 6 0 11.90 4.90 2 6 0 18.80 3.30 -2 6 0 25.90 7.30 -2 6 0 19.50 5.10 -2 6 0 21.90 2.30 -2 6 0 17.20 5.10 -2 6 0 30.70 3.90 -3 -6 0 -4.60 4.30 3 -6 0 1.50 3.50 3 -6 0 0.90 1.50 3 -6 0 -3.50 5.60 3 -6 0 -0.90 5.20 -3 -6 0 0.70 5.20 3 -6 0 -10.10 4.10 -3 -6 0 -6.30 6.60 3 6 0 6.00 4.10 -3 6 0 2.30 3.00 -3 6 0 -3.60 7.60 3 6 0 4.50 2.50 3 6 0 -2.50 2.90 -3 6 0 -1.80 1.40 -3 6 0 -5.70 5.80 3 6 0 -0.30 3.50 4 -6 0 4.20 6.90 -4 -6 0 -1.20 5.10 4 -6 0 -2.60 3.80 4 -6 0 -3.40 6.20 -4 -6 0 2.50 7.90 -4 -6 0 4.90 5.50 -4 6 0 -1.20 3.60 -4 6 0 3.90 7.60 4 6 0 -1.10 3.10 -4 6 0 20.80 8.90 4 6 0 12.60 8.00 4 6 0 -0.20 2.80 4 6 0 5.80 3.80 5 -6 0 2.20 4.40 -5 -6 0 8.00 5.80 -5 -6 0 6.20 8.80 -5 -6 0 -11.00 6.00 5 -6 0 -6.20 6.10 5 -6 0 -2.00 6.70 -5 6 0 6.10 7.80 -5 6 0 17.50 9.90 5 6 0 9.80 8.60 5 6 0 -1.20 4.30 5 6 0 -4.90 8.80 -6 -6 0 21.30 10.10 6 -6 0 8.40 8.30 6 -6 0 13.00 9.40 -6 -6 0 8.00 7.50 -6 -6 0 5.00 6.10 6 -6 0 13.00 6.10 6 6 0 -0.60 9.90 -6 6 0 2.20 9.20 6 6 0 15.50 11.70 6 6 0 12.60 6.70 6 6 0 12.30 5.00 -6 6 0 16.00 11.30 7 -6 0 0.00 9.50 -7 -6 0 -12.90 10.10 7 -6 0 -1.30 6.00 7 -6 0 10.30 10.00 -7 -6 0 9.60 8.60 7 6 0 14.70 12.10 7 6 0 10.90 6.30 -7 6 0 16.00 12.40 7 6 0 4.60 5.60 -7 6 0 15.00 10.20 7 6 0 4.30 12.20 -8 -6 0 -4.10 11.30 8 -6 0 16.90 11.50 -8 -6 0 -6.60 9.00 8 -6 0 9.60 11.60 8 6 0 -8.80 7.00 -8 6 0 8.00 10.60 8 6 0 6.90 14.90 -8 6 0 0.90 13.10 8 6 0 3.90 13.40 0 -7 0 -0.20 5.00 0 -7 0 5.60 4.70 0 -7 0 -4.90 3.20 0 7 0 -0.20 5.00 0 7 0 -2.60 2.50 0 7 0 4.60 5.00 0 7 0 3.70 3.10 0 7 0 -3.00 4.20 -1 -7 0 88.49 8.40 1 -7 0 111.99 9.70 -1 -7 0 112.19 7.80 1 -7 0 97.19 8.20 1 -7 0 102.29 7.40 1 7 0 95.39 6.20 -1 7 0 103.89 8.40 -1 7 0 101.39 5.70 -1 7 0 101.49 7.80 -1 7 0 94.09 10.50 -1 7 0 114.69 8.30 1 7 0 106.69 7.30 -1 7 0 94.39 10.90 -1 7 0 106.29 7.20 1 7 0 106.69 6.40 1 7 0 110.39 8.20 -1 7 0 90.29 7.40 -2 -7 0 4.50 5.10 2 -7 0 7.20 6.20 2 -7 0 -2.30 3.40 2 -7 0 1.80 5.90 -2 -7 0 3.30 4.20 -2 7 0 2.30 2.00 2 7 0 9.00 4.10 -2 7 0 -5.70 4.00 -2 7 0 -3.00 3.50 -2 7 0 4.30 5.60 -2 7 0 5.10 7.90 3 -7 0 13.00 4.40 3 -7 0 13.50 7.30 -3 -7 0 13.30 6.40 -3 -7 0 4.90 8.50 -3 -7 0 11.90 5.90 3 -7 0 22.70 6.60 -3 7 0 14.90 4.00 -3 7 0 8.60 6.70 -3 7 0 15.40 9.10 3 7 0 7.10 3.60 -4 -7 0 0.00 6.10 4 -7 0 8.60 7.60 -4 -7 0 2.70 5.80 4 -7 0 -4.80 7.20 4 -7 0 11.20 5.30 4 7 0 9.10 3.30 -4 7 0 9.00 8.20 -4 7 0 11.30 9.60 4 7 0 10.60 3.80 4 7 0 -3.10 9.40 4 7 0 1.60 4.50 -5 -7 0 197.88 12.60 5 -7 0 143.59 12.90 -5 -7 0 175.58 16.60 5 -7 0 179.18 12.30 -5 -7 0 175.08 13.60 5 -7 0 150.88 14.10 -5 7 0 191.28 14.40 -5 7 0 170.88 17.60 5 7 0 155.48 13.80 5 7 0 185.88 10.10 6 -7 0 12.80 6.30 -6 -7 0 14.10 9.10 -6 -7 0 -4.60 8.50 6 -7 0 17.60 9.00 -6 -7 0 27.80 7.10 6 -7 0 11.70 9.60 6 7 0 11.70 5.00 -6 7 0 24.10 10.00 -6 7 0 33.70 12.50 6 7 0 35.90 8.20 6 7 0 19.50 9.50 6 7 0 10.80 13.00 -7 -7 0 11.70 9.00 7 -7 0 19.60 6.50 -7 -7 0 21.70 11.50 7 -7 0 23.40 10.90 7 -7 0 15.40 9.10 -7 7 0 19.80 10.60 7 7 0 19.90 13.90 7 7 0 30.60 7.30 7 7 0 15.40 12.00 -7 7 0 16.60 13.20 8 -7 0 13.70 12.50 8 -7 0 26.60 7.50 8 -7 0 4.70 11.00 -8 -7 0 18.20 10.20 -8 -7 0 10.60 12.20 8 7 0 16.20 15.00 -8 7 0 57.19 16.70 8 7 0 34.90 8.30 -8 7 0 24.00 11.60 8 7 0 23.70 13.50 0 -8 0 31.10 7.00 0 -8 0 39.00 5.20 0 -8 0 54.99 7.00 0 8 0 45.70 7.00 0 8 0 42.20 5.40 0 8 0 31.80 5.60 0 8 0 38.50 5.10 -1 -8 0 78.99 9.90 -1 -8 0 87.29 8.20 1 -8 0 85.29 9.80 1 -8 0 87.39 10.00 1 -8 0 88.79 7.80 -1 8 0 79.09 5.50 1 8 0 86.39 6.00 1 8 0 62.99 7.10 -1 8 0 75.39 6.90 -1 8 0 74.69 8.30 -1 8 0 104.99 12.90 -1 8 0 78.79 9.50 2 -8 0 1.50 6.70 2 -8 0 2.70 3.90 -2 -8 0 1.50 5.20 2 -8 0 7.60 7.00 -2 8 0 8.60 2.60 -2 8 0 0.30 10.20 -2 8 0 -5.70 4.20 2 8 0 -3.30 3.10 2 8 0 5.30 4.20 -2 8 0 5.30 3.90 -2 8 0 -3.80 6.00 -3 -8 0 131.59 11.40 -3 -8 0 109.89 9.20 3 -8 0 108.69 11.00 3 -8 0 84.39 11.30 3 -8 0 121.09 9.20 3 8 0 119.39 7.60 -3 8 0 125.89 17.80 3 8 0 102.89 7.90 -3 8 0 93.89 10.50 -3 8 0 87.59 7.00 -4 -8 0 19.00 9.70 4 -8 0 19.50 8.90 4 -8 0 22.50 5.50 -4 -8 0 13.40 7.50 4 -8 0 37.50 9.20 -4 8 0 44.40 12.30 4 8 0 16.70 9.80 -5 -8 0 40.20 8.40 -5 -8 0 28.90 10.90 -5 -8 0 21.10 7.90 5 -8 0 42.30 7.30 5 -8 0 31.00 9.10 5 -8 0 49.20 10.40 5 8 0 23.90 8.80 -5 8 0 41.20 12.30 -5 8 0 32.40 9.10 5 8 0 26.00 10.50 5 8 0 40.70 8.40 6 -8 0 49.10 11.00 6 -8 0 39.50 10.20 -6 -8 0 56.69 9.80 -6 -8 0 71.49 12.60 6 -8 0 37.50 7.80 -6 8 0 43.20 13.20 -6 8 0 42.00 10.90 6 8 0 39.80 8.40 6 8 0 36.80 13.90 6 8 0 56.69 11.40 6 8 0 58.59 6.80 7 -8 0 2.90 10.40 7 -8 0 16.60 12.40 7 -8 0 9.30 7.00 -7 -8 0 -11.50 8.10 -7 -8 0 6.00 11.50 -7 8 0 -4.80 13.10 7 8 0 8.30 7.00 -7 8 0 5.40 10.80 7 8 0 0.50 13.60 0 -9 0 3.50 6.20 0 -9 0 -3.40 4.00 0 -9 0 -10.80 7.20 0 9 0 1.90 6.10 0 9 0 6.80 6.40 0 9 0 -8.90 5.30 0 9 0 0.70 4.30 1 -9 0 104.39 10.90 -1 -9 0 136.09 11.90 -1 -9 0 139.19 9.90 1 -9 0 94.69 10.00 -1 9 0 118.29 10.20 -1 9 0 130.89 11.40 2 -9 0 2.10 4.80 -2 -9 0 4.80 5.30 2 -9 0 -6.20 7.10 2 -9 0 -0.30 7.70 -2 9 0 0.10 4.20 -2 9 0 22.70 10.80 -2 9 0 -7.10 6.70 3 -9 0 32.70 9.10 -3 -9 0 26.10 6.60 3 -9 0 28.70 6.50 3 -9 0 27.20 9.00 3 9 0 33.30 4.90 -3 9 0 23.10 12.40 4 -9 0 89.19 12.90 -4 -9 0 102.79 12.50 4 -9 0 131.49 13.40 4 -9 0 97.29 11.10 -4 9 0 88.19 12.20 -4 9 0 91.49 13.10 4 9 0 108.69 8.20 4 9 0 79.89 11.90 -5 -9 0 -5.70 7.40 5 -9 0 9.90 10.40 -5 -9 0 -3.80 10.60 5 -9 0 -1.80 6.30 -5 -9 0 12.30 11.00 5 -9 0 -3.60 8.90 5 9 0 5.30 10.50 -5 9 0 3.70 11.80 5 9 0 2.70 6.30 -5 9 0 -9.80 9.20 5 9 0 5.90 4.20 -6 -9 0 23.80 8.90 6 -9 0 8.80 6.10 -6 -9 0 16.40 11.70 6 -9 0 25.20 11.10 6 -9 0 35.80 13.10 6 9 0 14.90 8.20 6 9 0 27.90 11.40 6 9 0 -0.70 12.00 -6 9 0 12.20 11.70 -6 9 0 5.90 13.10 7 9 0 3.20 12.00 0 -10 0 43.60 8.40 0 -10 0 39.00 9.40 0 10 0 33.60 7.60 0 10 0 43.00 9.20 0 10 0 29.30 10.00 1 -10 0 109.09 9.50 -1 -10 0 106.59 10.40 1 -10 0 128.39 11.60 1 -10 0 95.49 10.90 -1 10 0 91.09 13.80 -1 10 0 97.49 10.30 -2 -10 0 47.80 8.10 2 -10 0 38.30 9.50 2 -10 0 44.30 6.90 2 -10 0 59.39 10.40 -2 10 0 44.60 12.00 -2 10 0 43.20 7.90 -3 -10 0 9.20 6.40 3 -10 0 2.60 9.40 3 -10 0 -3.70 4.60 3 -10 0 7.10 8.80 -3 10 0 13.00 8.30 3 10 0 3.40 5.10 -3 10 0 12.10 11.90 -4 -10 0 64.89 9.50 4 -10 0 100.19 12.80 4 -10 0 52.09 11.60 4 -10 0 68.09 8.80 -4 10 0 85.39 13.70 4 10 0 66.39 9.10 -4 10 0 67.09 10.80 4 10 0 39.40 12.40 4 10 0 82.19 7.80 -5 -10 0 33.80 9.70 5 -10 0 42.70 11.70 5 -10 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589.24 23.20 -5 -1 3 586.84 20.20 5 -1 -3 588.84 20.90 5 -1 -3 587.34 23.20 5 -1 -3 560.84 22.10 5 -1 -3 603.24 22.70 5 -1 -3 548.25 21.30 -5 -1 3 588.84 23.00 5 -1 -3 600.74 21.50 5 -1 -3 550.24 22.80 -5 -1 3 581.84 23.00 5 1 -3 551.14 22.30 -5 1 3 562.84 20.70 5 1 -3 552.04 22.70 -5 1 3 596.44 23.60 -5 1 3 564.24 22.60 5 1 -3 584.74 20.10 5 1 -3 587.94 23.00 5 1 -3 570.94 21.90 5 1 -3 617.34 22.10 5 1 -3 530.25 22.10 -5 1 3 540.25 20.90 4 -1 -3 5.50 4.50 4 -1 -3 1.20 3.20 -4 -1 3 8.10 4.90 -4 -1 3 3.00 2.70 4 -1 -3 4.40 4.30 4 -1 -3 7.80 5.30 4 -1 -3 2.80 2.40 4 -1 -3 8.10 5.20 4 -1 -3 3.00 3.80 -4 -1 3 6.30 4.90 4 1 -3 9.90 3.80 -4 1 3 12.90 5.90 4 1 -3 7.70 4.00 4 1 -3 4.50 5.20 -4 1 3 10.90 5.00 4 1 -3 -3.00 4.50 4 1 -3 12.30 5.50 4 1 -3 7.60 1.90 4 1 -3 5.70 4.10 -4 1 3 5.80 2.30 -4 1 3 0.80 2.80 3 -1 -3 237.38 10.40 3 -1 -3 225.48 10.00 3 -1 -3 233.68 9.70 -3 -1 3 233.48 11.80 -3 -1 3 221.68 8.00 3 -1 -3 231.58 11.50 3 -1 -3 242.58 11.20 -3 -1 3 222.58 10.40 -3 -1 3 209.68 9.50 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9.00 -2 2 14 71.69 11.00 1 -2 -14 7.20 6.40 1 -2 -14 12.40 11.20 -1 -2 14 21.10 6.20 -1 -2 14 13.00 9.70 -1 2 14 8.20 9.60 1 2 -14 19.00 6.10 -1 2 14 30.30 7.70 1 2 -14 18.60 10.50 0 -2 -14 159.58 13.00 0 -2 14 151.08 20.90 0 -2 14 158.88 13.50 0 -2 -14 181.08 19.60 0 2 -14 183.18 12.20 0 2 14 152.58 15.00 0 2 14 165.78 17.80 1 -2 14 -4.10 9.40 1 2 14 7.50 11.20 5 -3 -14 1.20 7.90 -5 -3 14 9.10 10.00 5 3 -14 3.50 11.70 5 3 -14 3.20 5.80 -5 3 14 19.70 10.50 -4 -3 14 16.20 10.00 4 -3 -14 18.90 7.60 4 -3 -14 26.00 17.00 4 -3 -14 13.70 8.00 4 3 -14 18.40 7.00 4 3 -14 17.20 11.20 -4 3 14 6.30 6.40 4 3 -14 0.00 7.40 -4 3 14 27.60 10.90 3 -3 -14 -1.80 7.40 3 -3 -14 9.60 11.30 3 -3 -14 0.40 6.30 -3 -3 14 11.40 9.80 -3 3 14 1.50 5.80 3 3 -14 -4.20 6.40 3 3 -14 -0.70 9.70 -3 3 14 23.50 10.10 3 3 -14 6.40 6.20 2 -3 -14 141.79 17.80 2 -3 -14 123.49 11.80 -2 -3 14 123.29 17.30 2 -3 -14 133.49 12.30 2 3 -14 137.59 17.70 -2 3 14 116.19 12.30 2 3 -14 139.39 12.70 2 3 -14 127.69 11.20 1 -3 -14 21.30 7.20 -1 -3 14 30.20 10.60 1 -3 -14 28.60 11.50 1 3 -14 18.40 10.30 1 3 -14 14.50 7.50 1 3 -14 27.60 6.80 -1 3 14 7.10 10.10 -1 3 14 33.50 7.80 0 -3 14 -17.90 8.60 0 -3 14 4.50 5.70 0 -3 -14 1.00 5.40 0 -3 -14 18.00 11.60 0 3 -14 -2.60 4.70 0 3 14 -2.50 7.50 0 3 -14 5.70 11.10 0 3 14 -6.90 10.70 0 3 -14 10.30 7.70 4 -4 -14 34.10 9.00 -4 -4 14 25.10 11.30 -4 4 14 26.70 7.30 4 4 -14 47.20 12.90 -4 4 14 51.69 12.40 4 4 -14 26.00 8.30 4 4 -14 32.10 7.30 -3 -4 14 100.99 14.10 3 -4 -14 93.59 20.10 3 -4 -14 77.29 9.80 3 -4 -14 92.59 11.90 -3 4 14 90.29 11.10 3 4 -14 99.49 10.50 3 4 -14 74.09 10.30 3 4 -14 66.19 12.90 2 -4 -14 73.29 13.40 2 -4 -14 65.09 8.70 -2 -4 14 58.39 12.70 2 4 -14 84.09 10.50 2 4 -14 65.89 8.20 -2 4 14 66.09 9.30 2 4 -14 81.79 12.80 1 -4 -14 43.40 11.50 1 -4 -14 30.80 9.80 -1 -4 14 28.70 11.20 1 -4 -14 20.30 7.50 1 4 -14 20.40 8.30 -1 4 14 19.60 7.70 -3 0 15 0.20 10.30 3 0 -15 -4.20 12.00 3 0 -15 -5.40 5.10 2 0 -15 -9.70 10.90 2 0 -15 5.30 6.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 54409 _shelx_res_file ; TITL umt_dd1_bp_a.res in P2(1)/c umt_dd1_bp.res created by SHELXL-2018/3 at 19:59:33 on 31-Jul-2023 REM Old TITL UMT_DD1_BP in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.118, Rweak 0.006, Alpha 0.017 REM 0.609 for 106 systematic absences, Orientation as input REM Formula found by SHELXT: C9 N2 O2 CELL 0.71073 7.6327 9.5561 11.2899 90 104.095 90 ZERR 4 0.0005 0.0006 0.0007 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 32 28 12 8 EQIV $1 2-X,2-Y,1-Z L.S. 20 PLAN 1 SIZE 0.04 0.12 0.16 TEMP -173.15 CONF HTAB O2 O1_$1 BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.040400 0.460300 FVAR 0.85441 O1 4 0.937368 0.864493 0.405964 11.00000 0.03475 0.01633 = 0.01638 0.00016 0.01220 -0.00412 O2 4 0.907435 0.889845 0.597018 11.00000 0.03711 0.01583 = 0.01468 -0.00444 0.00960 -0.00604 H2 2 0.962247 0.978655 0.591139 11.00000 0.08314 N1 3 0.565870 0.349789 0.202856 11.00000 0.02972 0.01522 = 0.01808 -0.00177 0.00052 -0.00086 N2 3 0.506634 0.463632 0.159001 11.00000 0.02715 0.02365 = 0.01188 -0.00398 0.00550 0.00096 N3 3 0.436068 0.561019 0.113598 11.00000 0.04036 0.02925 = 0.02256 0.00349 0.00811 0.01175 C1 1 0.820398 0.673820 0.497767 11.00000 0.01501 0.01322 = 0.01263 0.00116 0.00277 0.00061 C2 1 0.812393 0.587661 0.396272 11.00000 0.01433 0.01529 = 0.01171 0.00191 0.00387 0.00054 AFIX 43 H2A 2 0.845507 0.623981 0.326465 11.00000 -1.20000 AFIX 0 C3 1 0.756374 0.449485 0.396976 11.00000 0.01370 0.01442 = 0.01382 -0.00052 0.00304 0.00164 C4 1 0.708772 0.397262 0.500812 11.00000 0.01569 0.01365 = 0.01857 0.00240 0.00463 -0.00132 AFIX 43 H4 2 0.671218 0.302652 0.502454 11.00000 -1.20000 AFIX 0 C5 1 0.716068 0.482684 0.601246 11.00000 0.01897 0.02026 = 0.01368 0.00303 0.00672 -0.00005 AFIX 43 H5 2 0.683240 0.446267 0.671121 11.00000 -1.20000 AFIX 0 C6 1 0.771064 0.621093 0.600261 11.00000 0.01767 0.01831 = 0.01188 -0.00101 0.00421 0.00084 AFIX 43 H6 2 0.775077 0.679528 0.668945 11.00000 -1.20000 AFIX 0 C7 1 0.891819 0.817560 0.496868 11.00000 0.01762 0.01534 = 0.01209 -0.00028 0.00278 0.00099 C8 1 0.749140 0.356505 0.288132 11.00000 0.02174 0.01539 = 0.01496 -0.00165 0.00549 -0.00018 AFIX 23 H8A 2 0.836393 0.391527 0.243022 11.00000 -1.20000 H8B 2 0.786820 0.260833 0.317165 11.00000 -1.20000 AFIX 0 HKLF 4 REM umt_dd1_bp_a.res in P2(1)/c REM wR2 = 0.1006, GooF = S = 1.029, Restrained GooF = 1.029 for all data REM R1 = 0.0408 for 1496 Fo > 4sig(Fo) and 0.0628 for all 1988 data REM 122 parameters refined using 0 restraints END WGHT 0.0403 0.4617 REM Highest difference peak 0.322, deepest hole -0.227, 1-sigma level 0.050 Q1 1 0.8573 0.7372 0.5000 11.00000 0.05 0.32 ; _shelx_res_checksum 13566 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 0.93737(15) 0.86449(11) 0.40596(9) 0.0215(3) Uani d 1 . . O O2 0.90744(16) 0.88984(12) 0.59702(9) 0.0220(3) Uani d 1 . . H H2 0.962(4) 0.979(3) 0.591(2) 0.083(9) Uiso d 1 . . N N1 0.56587(18) 0.34979(13) 0.20286(11) 0.0219(3) Uani d 1 . . N N2 0.50663(18) 0.46363(14) 0.15900(11) 0.0208(3) Uani d 1 . . N N3 0.4361(2) 0.56102(16) 0.11360(13) 0.0306(3) Uani d 1 . . C C1 0.82040(18) 0.67382(14) 0.49777(12) 0.0137(3) Uani d 1 . . C C2 0.81239(18) 0.58766(14) 0.39627(12) 0.0137(3) Uani d 1 . . H H2A 0.845507 0.623981 0.326465 0.016 Uiso calc 1 . . C C3 0.75637(18) 0.44948(15) 0.39698(12) 0.0140(3) Uani d 1 . . C C4 0.70877(19) 0.39726(15) 0.50081(13) 0.0159(3) Uani d 1 . . H H4 0.671218 0.302652 0.502454 0.019 Uiso calc 1 . . C C5 0.71607(19) 0.48268(15) 0.60125(13) 0.0172(3) Uani d 1 . . H H5 0.683240 0.446267 0.671121 0.021 Uiso calc 1 . . C C6 0.77106(19) 0.62109(15) 0.60026(12) 0.0159(3) Uani d 1 . . H H6 0.775077 0.679528 0.668945 0.019 Uiso calc 1 . . C C7 0.89182(19) 0.81756(15) 0.49687(12) 0.0152(3) Uani d 1 . . C C8 0.74914(19) 0.35650(15) 0.28813(12) 0.0172(3) Uani d 1 . . H H8A 0.836393 0.391527 0.243022 0.021 Uiso calc 1 . . H H8B 0.786820 0.260833 0.317165 0.021 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 0.0348(6) 0.0163(5) 0.0164(5) -0.0041(5) 0.0122(5) 0.0002(4) O2 0.0371(6) 0.0158(5) 0.0147(5) -0.0060(5) 0.0096(4) -0.0044(4) N1 0.0297(7) 0.0152(6) 0.0181(6) -0.0009(5) 0.0005(5) -0.0018(5) N2 0.0271(7) 0.0236(7) 0.0119(6) 0.0010(6) 0.0055(5) -0.0040(5) N3 0.0404(9) 0.0292(8) 0.0226(7) 0.0117(7) 0.0081(6) 0.0035(6) C1 0.0150(6) 0.0132(6) 0.0126(6) 0.0006(5) 0.0028(5) 0.0012(5) C2 0.0143(6) 0.0153(7) 0.0117(6) 0.0005(5) 0.0039(5) 0.0019(5) C3 0.0137(6) 0.0144(7) 0.0138(6) 0.0016(5) 0.0030(5) -0.0005(5) C4 0.0157(7) 0.0136(7) 0.0186(7) -0.0013(5) 0.0046(5) 0.0024(5) C5 0.0190(7) 0.0203(7) 0.0137(6) 0.0000(6) 0.0067(6) 0.0030(6) C6 0.0177(7) 0.0183(7) 0.0119(6) 0.0008(6) 0.0042(5) -0.0010(5) C7 0.0176(7) 0.0153(7) 0.0121(6) 0.0010(5) 0.0028(5) -0.0003(5) C8 0.0217(7) 0.0154(7) 0.0150(6) -0.0002(6) 0.0055(6) -0.0017(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 O2 H2 . . 111.0(17) ? N2 N1 C8 . . 114.49(12) ? N3 N2 N1 . . 172.89(16) ? C2 C1 C7 . . 118.90(12) ? C6 C1 C2 . . 119.97(13) ? C6 C1 C7 . . 121.03(12) ? C1 C2 H2A . . 119.8 ? C3 C2 C1 . . 120.44(12) ? C3 C2 H2A . . 119.8 ? C2 C3 C4 . . 119.11(12) ? C2 C3 C8 . . 120.42(12) ? C4 C3 C8 . . 120.46(12) ? C3 C4 H4 . . 119.8 ? C5 C4 C3 . . 120.49(13) ? C5 C4 H4 . . 119.8 ? C4 C5 H5 . . 119.8 ? C4 C5 C6 . . 120.40(13) ? C6 C5 H5 . . 119.8 ? C1 C6 H6 . . 120.2 ? C5 C6 C1 . . 119.59(13) ? C5 C6 H6 . . 120.2 ? O1 C7 O2 . . 122.59(13) ? O1 C7 C1 . . 121.19(12) ? O2 C7 C1 . . 116.21(12) ? N1 C8 C3 . . 113.18(12) ? N1 C8 H8A . . 108.9 ? N1 C8 H8B . . 108.9 ? C3 C8 H8A . . 108.9 ? C3 C8 H8B . . 108.9 ? H8A C8 H8B . . 107.8 ? 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 . 1.2446(17) ? O2 H2 . 0.96(3) ? O2 C7 . 1.3054(17) ? N1 N2 . 1.2345(18) ? N1 C8 . 1.4939(19) ? N2 N3 . 1.1333(19) ? C1 C2 . 1.4002(19) ? C1 C6 . 1.3953(19) ? C1 C7 . 1.479(2) ? C2 H2A . 0.9500 ? C2 C3 . 1.389(2) ? C3 C4 . 1.4010(19) ? C3 C8 . 1.5065(19) ? C4 H4 . 0.9500 ? C4 C5 . 1.387(2) ? C5 H5 . 0.9500 ? C5 C6 . 1.389(2) ? C6 H6 . 0.9500 ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? 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 O1 3_776 0.96(3) 1.68(3) 2.6334(15) 175(3) 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 N2 N1 C8 C3 . . . . 59.97(17) ? C1 C2 C3 C4 . . . . -0.3(2) ? C1 C2 C3 C8 . . . . -179.53(12) ? C2 C1 C6 C5 . . . . 0.7(2) ? C2 C1 C7 O1 . . . . 3.0(2) ? C2 C1 C7 O2 . . . . -175.56(13) ? C2 C3 C4 C5 . . . . 0.5(2) ? C2 C3 C8 N1 . . . . -95.73(15) ? C3 C4 C5 C6 . . . . -0.1(2) ? C4 C3 C8 N1 . . . . 85.04(16) ? C4 C5 C6 C1 . . . . -0.5(2) ? C6 C1 C2 C3 . . . . -0.3(2) ? C6 C1 C7 O1 . . . . 179.39(13) ? C6 C1 C7 O2 . . . . 0.8(2) ? C7 C1 C2 C3 . . . . 176.11(12) ? C7 C1 C6 C5 . . . . -175.65(13) ? C8 C3 C4 C5 . . . . 179.75(13) ? _cod_database_fobs_code 2022834