#------------------------------------------------------------------------------ #$Date: 2023-03-16 04:10:54 +0100 (Thu, 16 Mar 2023) $ #$Revision: 281907 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022702.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_2022702 loop_ _publ_author_name 'Aristov, Michael M.' 'Geng, Han' 'Harris, James W.' 'Berry, John F.' _publ_section_title ; Clarifying the structures of imidines: using crystallographic characterization to identify tautomers and localized systems of \p-bonding ; _journal_coeditor_code EP3031 _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first ; ; _journal_paper_doi 10.1107/S2053229623002036 _journal_volume 79 _journal_year 2023 _chemical_formula_moiety 'C4 H6 N2 O' _chemical_formula_sum 'C4 H6 N2 O' _chemical_formula_weight 98.11 _chemical_name_systematic ; 5-Amino-3,4-dihydro-2H-pyrrol-2-one ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _cell_angle_alpha 90 _cell_angle_beta 115.741(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.3685(5) _cell_length_b 8.0074(7) _cell_length_c 8.4211(9) _cell_measurement_reflns_used 2533 _cell_measurement_temperature 99.99 _cell_measurement_theta_max 71.553 _cell_measurement_theta_min 6.689 _cell_volume 447.56(7) _computing_cell_refinement ; SAINT-Plus (Bruker, 2016) ; _computing_data_collection ; APEX3 (Bruker, 2016) ; _computing_data_reduction ; SAINT-Plus (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 ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 99.99 _diffrn_detector 'charge-coupled device (CCD) area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '0.60\ \w and 0.6\ \f scans' _diffrn_radiation_monochromator 'equatorially mounted graphite' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_unetI/netI 0.0217 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 7398 _diffrn_reflns_theta_full 67.000 _diffrn_reflns_theta_max 72.029 _diffrn_reflns_theta_min 6.688 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 32.0 _diffrn_source_power 1.28 _diffrn_source_voltage 40.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_T_max 0.9154 _exptl_absorpt_correction_T_min 0.8529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 208 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.226 _refine_diff_density_min -0.180 _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 72 _refine_ls_number_reflns 886 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0331 _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^)+(0.0517P)^2^+0.1366P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.0888 _reflns_number_gt 775 _reflns_number_total 886 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ep3031sup1.cif _cod_data_source_block 3 _cod_database_code 2022702 _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 0.915 _shelx_estimated_absorpt_t_max 0.965 _shelx_hkl_file ; 1 0 0 -1.20 2.90 1 0 0 1.60 3.20 1 0 0 10.60 3.20 2 0 0 1033.80 29.90 2 0 0 1042.10 29.30 2 0 0 996.90 28.90 3 0 0 0.50 5.80 3 0 0 -2.10 5.60 3 0 0 4.30 5.70 4 0 0 399.46 23.70 4 0 0 422.96 24.80 4 0 0 421.96 24.50 5 0 0 23.50 13.30 -6 0 0 246.28 15.90 6 0 0 262.67 13.20 -6 0 0 237.68 14.90 6 0 0 249.88 11.40 6 0 0 250.67 13.30 7 0 0 -2.70 4.90 -7 0 0 2.00 6.50 -7 0 0 -1.10 6.40 7 0 0 -2.30 4.30 8 0 0 219.78 8.70 -8 0 0 150.88 9.10 0 -1 0 0.50 2.60 0 1 0 2.10 3.10 0 1 0 2.30 2.70 -1 -1 0 5866.21 109.49 1 -1 0 5783.42 111.19 1 -1 0 5554.34 110.99 1 -1 0 5793.42 109.59 1 1 0 5719.33 112.89 1 1 0 5711.33 111.29 2 -1 0 577.74 20.70 2 -1 0 614.74 22.40 2 -1 0 589.14 21.70 2 1 0 617.64 22.00 2 1 0 612.14 23.10 2 1 0 616.24 21.30 3 -1 0 9.40 6.30 -3 -1 0 0.00 4.10 3 -1 0 6.20 5.80 3 -1 0 -8.10 5.40 3 1 0 11.40 6.40 3 1 0 2.50 6.20 3 1 0 12.20 7.30 4 -1 0 559.54 28.40 4 -1 0 553.14 28.90 -4 -1 0 553.84 21.20 4 1 0 558.44 29.90 4 1 0 553.54 29.60 4 1 0 571.44 28.30 5 -1 0 90.89 17.90 5 1 0 80.89 19.50 -6 -1 0 38.00 11.20 6 -1 0 40.40 6.00 -6 -1 0 54.39 9.90 -6 -1 0 50.99 9.40 6 -1 0 31.10 6.70 -6 1 0 34.40 8.70 -6 1 0 44.00 9.00 6 1 0 36.70 7.30 6 1 0 38.90 6.80 7 -1 0 11.30 5.30 -7 -1 0 14.30 7.20 7 -1 0 6.10 4.20 -7 -1 0 17.60 7.40 -7 1 0 19.10 7.10 7 1 0 17.70 6.10 7 1 0 13.80 5.10 -7 1 0 22.40 7.80 8 -1 0 150.28 7.40 8 1 0 160.18 7.80 -8 1 0 172.98 11.30 8 1 0 168.18 7.40 -8 1 0 141.39 8.30 0 -2 0 651.63 20.80 0 2 0 643.64 21.10 0 2 0 643.64 22.60 1 -2 0 631.84 21.10 -1 -2 0 645.44 21.00 1 -2 0 623.54 21.70 1 -2 0 646.14 23.10 1 2 0 653.83 22.30 1 2 0 622.14 23.90 2 -2 0 1405.26 40.80 -2 -2 0 1358.76 34.50 2 -2 0 1447.16 41.70 2 -2 0 1382.66 38.20 2 2 0 1424.96 41.70 2 2 0 1436.06 38.90 2 2 0 1439.66 43.70 3 -2 0 51.59 11.50 3 -2 0 49.10 10.80 -3 -2 0 61.69 8.60 3 -2 0 53.99 10.20 3 2 0 66.39 11.10 3 2 0 53.19 12.20 3 2 0 50.79 6.80 3 2 0 57.99 12.60 -4 -2 0 90.19 11.30 4 -2 0 69.59 14.40 4 -2 0 72.09 14.20 4 2 0 70.39 8.30 -4 2 0 76.69 6.10 4 2 0 81.99 16.20 4 2 0 81.89 16.00 -5 -2 0 20.30 8.50 5 -2 0 14.00 13.50 -5 -2 0 36.30 8.10 5 -2 0 38.60 6.90 5 -2 0 26.50 5.60 -5 -2 0 25.10 8.90 5 -2 0 29.80 9.30 -5 2 0 27.80 4.90 5 2 0 33.30 7.60 5 2 0 33.10 6.20 -5 2 0 30.60 8.50 6 -2 0 50.49 7.50 -6 -2 0 54.99 11.10 -6 -2 0 48.60 9.20 -6 -2 0 56.09 9.70 6 -2 0 42.20 6.20 -6 2 0 55.29 10.10 6 2 0 40.50 6.60 -6 2 0 44.80 9.30 6 2 0 49.00 7.80 7 -2 0 9.90 4.50 -7 -2 0 13.80 6.80 7 -2 0 19.30 5.70 7 2 0 19.80 5.50 7 2 0 23.20 6.00 -7 2 0 28.60 8.70 -7 2 0 22.40 7.40 -8 -2 0 36.40 5.10 8 2 0 36.90 4.10 0 -3 0 -9.30 4.70 0 3 0 2.80 6.90 0 3 0 2.30 6.40 1 -3 0 1.20 5.60 -1 -3 0 -1.60 4.80 1 -3 0 2.10 5.60 -1 -3 0 -3.20 3.70 -1 3 0 7.40 6.80 1 3 0 3.20 5.90 1 3 0 6.40 6.90 2 -3 0 184.98 16.40 -2 -3 0 195.78 11.30 2 -3 0 194.28 18.30 -2 -3 0 196.38 14.10 2 3 0 224.38 18.20 2 3 0 204.08 19.00 -2 3 0 202.98 17.40 2 3 0 194.58 10.60 3 -3 0 176.38 19.70 3 -3 0 195.08 20.50 3 -3 0 158.48 17.10 -3 -3 0 183.98 12.20 3 3 0 152.08 20.30 3 3 0 147.69 16.50 3 3 0 172.58 20.70 3 3 0 179.18 10.70 4 -3 0 16.10 10.60 -4 -3 0 5.10 6.20 4 3 0 6.40 11.40 -4 3 0 2.60 3.70 4 3 0 -9.70 10.40 4 3 0 2.30 3.10 4 3 0 3.80 4.70 5 -3 0 753.62 23.50 -5 -3 0 778.82 32.20 5 -3 0 780.52 21.80 5 -3 0 789.62 27.60 5 -3 0 791.72 23.50 -5 -3 0 766.92 29.30 -5 -3 0 780.42 27.20 5 3 0 800.42 24.40 -5 3 0 776.42 20.00 -5 3 0 753.02 24.90 -5 3 0 755.72 27.40 5 3 0 763.62 27.90 -6 -3 0 165.38 13.50 6 -3 0 148.39 9.30 6 -3 0 156.78 11.40 6 -3 0 140.39 10.40 -6 -3 0 135.89 13.60 -6 3 0 165.68 13.10 6 3 0 152.78 11.30 -6 3 0 146.69 13.70 -7 -3 0 39.20 8.10 -7 -3 0 38.70 7.70 7 -3 0 29.60 4.90 7 -3 0 31.50 5.60 -7 3 0 49.10 8.50 -7 3 0 37.80 7.30 7 3 0 38.20 5.90 0 -4 0 718.73 21.90 0 -4 0 767.92 31.00 0 4 0 718.03 30.40 0 4 0 719.73 33.90 -1 -4 0 191.98 11.70 -1 -4 0 189.78 18.00 1 -4 0 179.98 18.70 -1 4 0 196.08 21.00 1 4 0 195.78 10.40 1 4 0 191.78 21.70 -1 4 0 208.18 19.30 1 4 0 195.58 19.50 -2 -4 0 41.70 8.20 -2 -4 0 47.80 10.80 2 -4 0 44.10 11.00 2 4 0 36.70 6.30 2 4 0 42.40 13.20 -2 4 0 35.80 10.90 2 4 0 4.00 10.40 -2 4 0 38.30 12.20 3 -4 0 325.77 27.70 -3 -4 0 353.56 18.70 3 -4 0 330.27 25.50 3 4 0 380.26 29.70 -3 4 0 360.26 28.90 3 4 0 393.16 16.90 -3 4 0 356.16 11.60 3 4 0 372.06 27.50 3 4 0 351.26 10.40 4 -4 0 738.13 40.30 4 -4 0 646.54 22.10 -4 -4 0 707.03 27.40 -4 -4 0 717.03 25.40 -4 -4 0 740.03 30.30 4 -4 0 674.93 25.10 -4 -4 0 753.12 25.50 4 -4 0 714.73 22.10 4 4 0 705.33 17.20 -4 4 0 683.03 18.70 4 4 0 763.32 27.10 -5 -4 0 -0.30 8.10 5 -4 0 2.90 5.00 -5 -4 0 -3.20 6.10 5 -4 0 -0.60 4.30 5 -4 0 0.80 8.20 -5 -4 0 6.70 8.30 5 4 0 -0.70 5.00 5 4 0 12.40 6.40 -5 4 0 -1.00 4.20 -5 4 0 1.60 5.30 5 4 0 2.90 5.10 -5 4 0 7.80 7.70 6 -4 0 459.65 16.80 -6 -4 0 481.55 20.40 6 -4 0 473.85 16.00 -6 -4 0 450.65 21.50 6 4 0 428.16 17.30 -6 4 0 471.65 20.70 6 4 0 413.16 20.80 6 4 0 456.05 17.20 -7 -4 0 36.20 6.60 7 -4 0 54.09 5.50 -7 -4 0 38.30 7.10 -7 4 0 52.79 8.20 7 4 0 42.70 5.40 -7 4 0 32.10 6.10 0 -5 0 12.40 8.50 0 5 0 6.50 10.60 0 5 0 27.50 11.50 -1 -5 0 526.95 28.90 1 -5 0 508.05 29.70 -1 -5 0 524.05 21.70 1 5 0 529.35 19.30 -1 5 0 551.24 15.10 -1 5 0 550.44 34.10 1 5 0 474.55 28.90 1 5 0 498.85 13.50 -1 5 0 521.15 30.00 1 5 0 564.24 35.90 2 -5 0 741.03 37.90 -2 -5 0 780.02 29.40 -2 5 0 818.12 42.60 -2 5 0 737.43 37.30 2 5 0 677.13 38.90 2 5 0 746.53 43.30 2 5 0 730.53 17.90 -2 5 0 760.62 18.80 2 5 0 777.22 25.90 3 -5 0 2.40 10.80 -3 -5 0 1.40 4.90 -3 5 0 3.60 3.90 3 5 0 -0.40 14.00 3 5 0 1.70 2.90 3 5 0 1.00 5.00 4 -5 0 7.20 4.70 -4 -5 0 5.70 6.60 4 -5 0 6.50 7.70 -4 -5 0 18.90 7.60 4 -5 0 10.70 5.70 4 -5 0 7.50 7.30 -4 -5 0 10.50 7.90 4 -5 0 2.90 4.30 -4 -5 0 7.80 7.50 -4 5 0 10.10 4.30 4 5 0 13.30 6.10 -4 5 0 14.90 6.30 4 5 0 18.10 6.70 -5 -5 0 211.98 16.80 5 -5 0 192.18 12.00 5 -5 0 218.38 11.20 5 -5 0 218.78 11.10 -5 -5 0 192.98 17.80 -5 -5 0 206.68 15.30 5 -5 0 222.08 16.10 -5 5 0 207.08 13.20 5 5 0 216.28 13.70 5 5 0 227.18 16.70 -5 5 0 229.08 16.20 5 5 0 212.28 12.10 6 -5 0 -2.60 4.10 -6 -5 0 -5.80 5.80 -6 -5 0 -1.00 6.90 6 -5 0 -2.10 4.50 -6 5 0 2.60 4.80 -6 5 0 -5.00 6.90 6 5 0 -0.30 4.60 -6 5 0 0.00 5.70 6 5 0 2.10 4.10 7 -5 0 29.10 3.40 -7 -5 0 22.10 5.70 -7 5 0 42.00 5.70 0 -6 0 0.80 10.70 0 6 0 2.90 11.40 0 6 0 -0.70 2.70 0 6 0 -3.90 14.00 -1 -6 0 382.36 20.50 -1 -6 0 352.66 28.40 1 -6 0 406.46 31.00 1 6 0 405.36 17.90 -1 6 0 343.47 35.60 -1 6 0 389.26 12.40 1 6 0 304.27 35.20 1 6 0 395.76 12.10 -2 -6 0 103.29 12.00 -2 -6 0 106.19 10.10 2 -6 0 100.09 11.80 -2 -6 0 113.89 10.00 -2 -6 0 113.19 14.60 2 -6 0 104.29 11.10 -2 -6 0 124.49 13.40 2 -6 0 101.59 10.40 2 -6 0 111.69 9.40 2 6 0 116.19 6.70 2 6 0 106.49 11.60 2 6 0 102.39 9.70 -2 6 0 110.19 7.40 3 -6 0 0.50 4.90 3 -6 0 9.90 7.20 -3 -6 0 0.10 7.10 3 -6 0 2.70 7.60 -3 -6 0 4.10 5.80 -3 -6 0 8.40 7.80 -3 -6 0 -1.00 7.10 3 -6 0 2.30 5.20 3 6 0 -2.50 5.50 -3 6 0 3.60 4.30 -3 6 0 4.30 4.40 3 6 0 1.60 3.20 3 6 0 1.20 4.70 -4 -6 0 -5.40 8.10 -4 -6 0 -5.90 6.50 4 -6 0 3.20 4.40 4 -6 0 -2.60 5.40 -4 -6 0 -9.40 7.70 -4 -6 0 -12.50 5.30 4 -6 0 -1.90 8.40 4 6 0 -1.80 4.70 4 6 0 -3.40 5.80 -4 6 0 5.90 6.50 -4 6 0 3.70 4.40 5 -6 0 35.80 6.90 -5 -6 0 54.69 10.80 5 -6 0 36.30 5.80 -5 -6 0 35.00 8.40 5 -6 0 25.70 5.00 -5 6 0 40.30 7.10 5 6 0 25.30 7.60 -5 6 0 45.00 9.60 5 6 0 20.50 5.50 -6 -6 0 43.10 6.40 6 -6 0 32.10 4.90 6 -6 0 57.59 5.20 -6 -6 0 53.59 8.10 6 6 0 54.09 5.90 -6 6 0 55.29 7.80 0 -7 0 -2.40 4.60 0 -7 0 -7.50 4.70 0 -7 0 1.50 6.10 0 -7 0 -1.20 7.00 0 7 0 0.50 3.50 0 7 0 0.70 3.90 1 -7 0 268.57 13.30 1 -7 0 271.87 14.90 1 -7 0 288.97 19.20 -1 -7 0 274.77 15.00 1 -7 0 256.27 16.80 -1 -7 0 272.67 18.00 -1 -7 0 253.07 13.60 1 -7 0 263.77 13.00 1 7 0 260.87 10.30 -1 7 0 249.97 10.40 -2 -7 0 21.40 9.60 2 -7 0 20.30 6.30 2 -7 0 27.20 7.30 -2 -7 0 16.30 5.60 2 -7 0 29.60 8.90 2 -7 0 21.00 8.60 -2 -7 0 14.10 7.90 -2 -7 0 12.30 8.00 -2 7 0 19.10 5.00 2 7 0 10.90 4.00 2 7 0 18.10 7.30 -2 7 0 15.10 5.10 2 7 0 12.00 5.70 -3 -7 0 46.70 12.10 -3 -7 0 48.20 10.30 -3 -7 0 29.20 7.50 3 -7 0 43.90 7.50 3 -7 0 40.10 8.90 3 -7 0 43.90 6.80 -3 -7 0 50.19 9.60 3 7 0 56.99 7.70 -3 7 0 39.50 5.70 3 7 0 39.70 9.40 -3 7 0 37.60 5.60 4 -7 0 196.58 15.70 -4 -7 0 182.58 13.80 -4 -7 0 220.78 16.40 4 -7 0 176.48 10.60 4 -7 0 197.28 11.80 4 7 0 200.28 12.60 4 7 0 186.38 14.40 -4 7 0 192.48 12.30 4 7 0 183.88 10.40 5 -7 0 16.50 4.30 5 -7 0 11.50 4.60 -5 -7 0 12.60 5.50 -5 -7 0 12.70 6.50 -5 7 0 19.00 6.50 5 7 0 21.90 5.30 -5 7 0 12.00 4.70 0 -8 0 13.00 6.40 0 -8 0 17.70 6.40 0 -8 0 17.50 9.10 0 -8 0 18.20 8.30 0 8 0 13.10 4.30 0 8 0 8.60 4.90 -1 -8 0 15.60 6.00 1 -8 0 7.80 7.30 1 -8 0 7.80 5.40 -1 -8 0 7.80 8.00 -1 -8 0 11.50 8.00 1 -8 0 4.80 7.90 1 8 0 8.30 4.00 -1 8 0 7.70 4.30 -1 8 0 9.50 5.50 1 8 0 5.40 4.40 -2 -8 0 30.70 7.10 2 -8 0 22.80 7.20 2 -8 0 22.70 8.10 2 -8 0 21.80 5.90 -2 -8 0 21.20 8.80 -2 8 0 19.40 5.40 2 8 0 16.90 4.80 -2 8 0 12.90 4.60 3 -8 0 919.11 27.70 3 -8 0 912.11 24.20 3 -8 0 917.91 24.60 -3 -8 0 991.80 32.00 -3 8 0 939.31 23.50 3 8 0 914.51 25.10 -3 8 0 954.20 26.80 3 8 0 957.00 24.90 4 -8 0 87.69 7.20 -4 -8 0 76.39 9.90 4 -8 0 89.29 7.40 -4 8 0 88.49 9.80 4 8 0 90.69 8.50 -4 8 0 80.49 7.30 4 8 0 75.39 6.40 0 -9 0 -0.50 4.80 0 -9 0 -0.40 7.10 0 -9 0 0.60 5.60 0 9 0 2.30 4.10 0 9 0 2.60 4.80 1 -9 0 132.39 8.50 -1 -9 0 117.79 12.20 -1 9 0 136.39 9.10 1 9 0 130.49 8.80 1 9 0 136.99 8.50 -2 -9 0 140.99 11.70 2 -9 0 136.29 8.30 -2 9 0 133.59 9.00 2 9 0 150.28 8.40 -2 9 0 146.09 8.60 2 9 0 146.39 8.20 -3 -9 0 107.39 9.60 3 -9 0 84.99 6.10 3 9 0 98.29 6.20 -3 9 0 91.89 6.30 -8 0 1 2.40 5.60 8 0 -1 -2.50 4.20 -8 0 1 -5.40 6.20 -7 0 1 116.89 12.50 -7 0 1 98.69 11.30 7 0 -1 112.59 9.90 7 0 -1 92.69 9.40 -6 0 1 -1.30 6.20 6 0 -1 0.10 4.70 -6 0 1 1.70 6.40 6 0 -1 3.80 4.90 5 0 -1 17.60 11.50 4 0 -1 -6.20 6.30 4 0 -1 5.00 7.70 3 0 -1 9999.00 196.88 3 0 -1 9765.02 189.18 3 0 -1 9957.50 191.28 2 0 -1 0.90 3.10 2 0 -1 3.40 5.50 2 0 -1 -2.10 3.90 1 0 -1 256.67 10.50 1 0 -1 253.27 7.20 0 0 1 4.80 2.40 0 0 1 1.30 2.20 0 0 1 -0.50 1.40 1 0 1 1078.99 29.10 1 0 1 1080.39 30.80 1 0 1 1121.19 25.40 2 0 1 1.60 4.70 2 0 1 -1.80 4.40 2 0 1 0.70 5.00 3 0 1 175.58 13.80 3 0 1 201.98 19.30 3 0 1 230.88 18.80 4 0 1 4.20 10.00 4 0 1 9.90 9.90 -4 0 -1 0.60 3.10 -5 0 -1 596.54 23.00 5 0 1 670.93 26.50 5 0 1 672.03 18.90 5 0 1 670.03 21.30 5 0 1 683.73 21.80 -5 0 -1 671.43 24.60 6 0 1 2.90 5.20 -6 0 -1 0.50 8.50 -6 0 -1 8.90 7.10 6 0 1 3.50 4.80 6 0 1 5.40 4.30 -6 0 -1 5.20 6.80 -7 0 -1 34.50 7.20 7 0 1 32.20 5.70 -8 -1 1 13.20 5.70 8 -1 -1 16.80 5.20 -8 -1 1 16.10 6.70 -8 1 1 17.70 5.60 -8 1 1 21.90 6.90 8 1 -1 12.50 4.10 8 1 -1 18.20 4.90 -7 -1 1 113.69 12.60 7 -1 -1 86.39 7.40 -7 -1 1 107.79 11.60 7 -1 -1 94.99 9.60 -7 1 1 107.49 12.00 7 1 -1 102.79 10.30 -7 1 1 105.09 11.80 7 1 -1 106.59 10.40 -6 -1 1 428.76 19.70 6 -1 -1 409.16 14.60 -6 -1 1 382.66 18.30 6 -1 -1 438.86 17.80 6 1 -1 422.06 17.00 -6 1 1 402.86 19.20 -6 1 1 429.76 20.20 6 1 -1 408.06 16.60 5 -1 -1 290.37 28.50 5 1 -1 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7.50 -5 2 -4 3.60 3.70 5 2 4 12.30 4.60 -5 2 -4 12.80 6.30 5 2 4 13.00 5.00 -8 -3 4 108.99 10.60 8 -3 -4 98.59 7.30 -8 -3 4 91.39 7.50 -8 -3 4 73.99 9.30 -8 3 4 100.19 9.50 8 3 -4 112.89 8.40 -8 3 4 89.19 8.10 -7 -3 4 0.70 6.80 -7 -3 4 9.30 7.10 -7 -3 4 3.50 5.90 -7 -3 4 7.10 6.10 7 -3 -4 3.30 5.20 7 -3 -4 9.00 6.40 -7 -3 4 6.10 13.10 7 3 -4 8.80 5.80 -7 3 4 5.90 5.50 -7 3 4 7.90 7.80 7 3 -4 8.00 7.40 -6 -3 4 173.98 12.90 -6 -3 4 169.88 10.30 -6 -3 4 187.98 13.80 -6 -3 4 173.08 12.40 6 -3 -4 175.78 10.20 -6 -3 4 185.48 15.40 -6 -3 4 173.08 16.70 -6 -3 4 195.38 11.60 -6 -3 4 188.38 12.10 -6 3 4 191.38 12.30 -6 3 4 198.78 10.70 6 3 -4 180.08 8.40 5 -3 -4 94.69 6.30 -5 -3 4 89.29 8.50 -5 -3 4 97.19 11.40 -5 -3 4 87.69 8.50 5 -3 -4 55.19 19.80 5 -3 -4 92.69 9.00 -5 -3 4 95.69 9.70 -5 -3 4 99.69 10.10 -5 -3 4 77.19 12.90 -5 -3 4 100.19 11.80 -5 -3 4 94.99 9.60 -5 -3 4 95.29 12.00 5 -3 -4 93.29 8.20 -5 3 4 99.49 9.80 -5 3 4 89.29 9.30 5 3 -4 87.69 5.90 -5 3 4 97.69 8.50 4 -3 -4 152.78 20.70 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8.60 -3 -3 -4 8.50 8.00 3 -3 4 11.90 5.30 3 -3 4 9.40 4.70 -3 -3 -4 3.20 3.90 3 -3 4 12.80 4.70 3 3 4 8.60 6.20 -3 3 -4 9.90 4.70 3 3 4 8.00 4.90 3 3 4 6.90 5.10 3 3 4 6.20 5.50 4 -3 4 123.49 9.90 -4 -3 -4 122.69 13.30 4 -3 4 118.69 12.20 4 -3 4 122.19 12.90 4 -3 4 121.09 8.90 4 -3 4 112.69 8.60 4 3 4 122.59 9.90 -4 3 -4 124.69 8.30 4 3 4 103.79 9.80 -5 -3 -4 11.40 6.50 5 -3 4 11.30 4.00 5 -3 4 9.30 7.00 5 -3 4 18.40 5.30 5 -3 4 16.90 4.00 -5 3 -4 15.70 3.80 5 3 4 16.40 4.50 5 3 4 13.40 4.20 -5 3 -4 10.60 5.50 -8 -4 4 8.50 5.60 8 -4 -4 2.40 3.80 -8 -4 4 3.00 4.10 8 4 -4 5.70 3.70 -8 4 4 16.50 4.30 8 4 -4 5.90 3.60 -7 -4 4 90.79 9.20 -7 -4 4 75.79 10.30 -7 -4 4 85.09 9.20 -7 -4 4 59.69 8.80 -7 -4 4 87.39 7.80 7 -4 -4 63.69 6.80 7 4 -4 86.29 8.80 7 4 -4 87.09 5.80 7 4 -4 57.09 9.70 -7 4 4 59.89 7.70 -6 -4 4 10.60 5.80 6 -4 -4 18.10 6.80 -6 -4 4 14.50 7.80 -6 -4 4 3.90 5.00 -6 -4 4 12.30 7.60 -6 -4 4 7.70 5.30 -6 -4 4 8.40 5.90 6 -4 -4 12.60 5.30 -6 -4 4 11.90 8.10 -6 4 4 10.50 5.30 6 4 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-4 323.87 19.30 0 4 -4 308.47 30.50 0 4 4 269.37 29.60 0 4 4 288.57 15.60 0 4 -4 247.68 29.70 1 -4 4 116.59 12.70 1 -4 4 105.69 8.90 1 -4 4 166.48 13.70 -1 -4 -4 100.19 6.90 1 -4 4 106.29 13.30 1 -4 4 56.79 20.80 -1 -4 -4 98.99 13.90 1 4 4 109.89 11.70 1 4 4 95.99 8.80 1 4 4 94.59 9.40 1 4 4 79.39 20.60 -2 -4 -4 15.20 9.00 -2 -4 -4 5.30 7.90 2 -4 4 6.70 5.10 2 -4 4 14.10 8.70 2 -4 4 19.70 6.40 2 -4 4 9.30 7.70 2 -4 4 10.10 4.50 2 -4 4 9.20 7.60 2 4 4 11.00 5.30 2 4 4 16.10 6.00 2 4 4 15.30 6.50 2 4 4 9.70 4.90 3 -4 4 93.79 13.60 3 -4 4 94.39 15.80 3 -4 4 97.29 12.70 -3 -4 -4 60.09 10.90 3 -4 4 91.19 8.20 -3 -4 -4 89.39 14.50 3 -4 4 83.79 9.00 3 -4 4 72.89 7.80 3 4 4 53.89 8.70 -3 4 -4 88.39 7.60 3 4 4 81.89 9.10 3 4 4 80.29 8.50 4 -4 4 -2.20 4.10 4 -4 4 1.40 4.70 -4 -4 -4 0.40 7.40 4 -4 4 -0.70 7.20 4 -4 4 -2.60 6.80 4 -4 4 3.10 4.20 -4 4 -4 -2.20 3.70 4 4 4 -1.10 4.30 -5 -4 -4 26.10 6.50 5 -4 4 9.40 5.10 5 -4 4 11.20 3.60 5 -4 4 9.50 3.30 5 -4 4 10.70 2.80 5 4 4 17.80 4.10 -5 4 -4 9.60 4.40 -7 -5 4 63.19 7.90 -7 -5 4 73.39 7.70 -7 -5 4 57.99 8.60 -7 -5 4 49.20 6.30 7 -5 -4 58.99 6.20 -7 -5 4 57.09 5.90 7 -5 -4 65.99 6.80 7 5 -4 75.49 5.60 -7 5 4 43.40 6.00 -6 -5 4 -6.30 6.80 -6 -5 4 1.10 5.90 -6 -5 4 7.30 6.20 -6 -5 4 -0.60 4.50 6 -5 -4 -3.00 4.50 -6 -5 4 3.10 5.60 6 -5 -4 -1.90 5.70 -6 -5 4 -0.70 6.80 6 5 -4 -5.20 6.30 6 5 -4 0.30 3.00 -6 5 4 4.30 5.50 -6 5 4 -2.50 4.50 5 -5 -4 85.79 8.50 -5 -5 4 94.29 10.50 5 -5 -4 75.99 8.80 -5 -5 4 95.39 9.30 -5 -5 4 69.89 8.70 -5 -5 4 76.99 10.50 -5 -5 4 84.89 8.60 -5 -5 4 77.99 11.10 -5 -5 4 60.59 12.70 5 5 -4 64.39 10.70 -5 5 4 92.29 9.40 -5 5 4 88.89 8.60 5 5 -4 83.39 6.10 -4 -5 4 282.97 15.50 -4 -5 4 301.97 14.00 -4 -5 4 290.37 13.90 -4 -5 4 280.57 20.90 -4 -5 4 280.97 14.80 4 -5 -4 287.57 12.40 4 -5 -4 276.47 12.80 -4 -5 4 307.17 17.40 -4 -5 4 282.97 16.80 4 -5 -4 295.97 14.80 -4 5 4 299.97 15.00 -4 5 4 275.17 12.90 -4 5 4 271.77 12.80 4 5 -4 284.97 9.80 4 5 -4 277.57 18.20 -3 -5 4 104.29 12.20 3 -5 -4 122.89 9.50 -3 -5 4 144.39 13.90 -3 -5 4 116.29 9.50 -3 -5 4 134.19 13.00 -3 -5 4 124.69 10.10 -3 -5 4 103.39 15.00 3 -5 -4 128.39 10.50 -3 -5 4 135.59 11.20 3 5 -4 113.79 12.80 -3 5 4 120.59 9.60 -3 5 4 123.19 9.10 2 -5 -4 111.99 9.20 -2 -5 4 117.39 11.90 -2 -5 4 96.89 20.40 -2 -5 4 121.09 9.40 -2 -5 4 92.69 18.50 -2 -5 4 130.39 12.60 2 -5 -4 131.49 15.00 -2 -5 4 120.49 10.70 2 5 -4 108.59 23.50 -2 5 4 126.79 12.40 -2 5 4 131.39 11.10 -2 5 4 126.99 9.20 1 -5 -4 2.60 6.40 -1 -5 4 1.20 6.20 -1 -5 4 2.70 5.60 -1 -5 4 5.50 6.70 -1 -5 4 2.10 7.50 1 -5 -4 -3.20 4.30 -1 -5 4 8.60 12.90 -1 5 4 -4.20 3.90 -1 5 4 2.10 4.70 1 5 -4 0.10 14.00 -1 5 4 1.70 4.80 0 -5 4 197.68 14.30 0 -5 -4 194.58 16.40 0 -5 4 195.48 16.30 0 -5 -4 183.28 11.30 0 -5 4 178.68 14.20 0 -5 4 173.98 11.90 0 -5 4 179.48 10.50 0 5 4 187.28 12.40 0 5 4 189.48 10.90 0 5 4 190.48 13.70 -1 -5 -4 801.12 33.70 1 -5 4 794.42 28.20 1 -5 4 844.72 29.20 1 -5 4 831.92 24.20 1 -5 4 837.72 24.10 1 -5 4 812.92 31.00 1 5 4 813.22 25.10 1 5 4 843.32 29.80 1 5 4 820.82 23.80 -2 -5 -4 601.34 25.50 2 -5 4 611.24 20.20 2 -5 4 592.74 19.80 -2 -5 -4 615.44 29.30 2 -5 4 631.74 26.90 2 -5 4 630.94 25.10 2 -5 4 579.74 23.80 2 5 4 610.24 20.00 2 5 4 608.44 21.00 -2 5 -4 611.24 17.40 2 5 4 630.64 25.00 3 -5 4 3.10 5.00 3 -5 4 8.30 5.20 -3 -5 -4 4.30 8.30 3 -5 4 11.30 8.80 3 -5 4 12.90 8.40 3 -5 4 9.70 8.40 -3 5 -4 9.60 4.70 3 5 4 8.50 5.10 3 5 4 10.40 5.70 3 5 4 10.60 6.30 4 -5 4 1.80 3.60 4 -5 4 -1.10 6.50 4 -5 4 0.50 4.00 -4 -5 -4 0.10 6.40 4 -5 4 4.20 3.60 4 -5 4 1.50 7.20 4 5 4 1.70 3.90 4 5 4 1.00 4.20 -4 5 -4 2.20 7.70 -4 5 -4 0.50 3.50 -7 -6 4 374.36 14.10 -7 -6 4 444.86 14.80 7 -6 -4 419.76 11.40 7 -6 -4 440.96 13.30 -7 6 4 369.46 12.60 7 6 -4 424.46 13.00 -6 -6 4 51.29 7.20 -6 -6 4 34.90 5.70 -6 -6 4 26.80 8.10 -6 -6 4 29.50 6.40 6 -6 -4 35.30 6.00 -6 -6 4 44.50 6.40 -6 -6 4 35.40 8.10 6 -6 -4 27.10 6.00 -6 6 4 30.90 6.00 6 6 -4 34.60 4.20 -6 6 4 49.99 6.30 5 -6 -4 1.10 5.70 -5 -6 4 0.70 6.20 -5 -6 4 0.70 7.00 5 -6 -4 -2.30 4.70 -5 -6 4 3.80 5.70 -5 -6 4 0.40 4.60 -5 -6 4 -1.50 5.70 -5 -6 4 -6.00 7.40 -5 6 4 1.20 5.50 -5 6 4 2.30 5.20 5 6 -4 -5.00 6.20 5 6 -4 -4.30 2.90 -4 -6 4 10.10 5.50 -4 -6 4 0.70 6.70 -4 -6 4 15.70 10.00 4 -6 -4 9.30 4.60 4 -6 -4 4.40 6.00 -4 -6 4 7.80 8.40 -4 -6 4 4.10 6.30 -4 -6 4 -0.80 5.20 -4 -6 4 3.70 6.50 -4 -6 4 3.10 7.10 -4 6 4 1.50 4.90 -4 6 4 4.90 5.80 4 6 -4 8.50 7.70 -4 6 4 10.30 4.90 4 6 -4 8.90 3.30 3 -6 -4 5.00 4.90 -3 -6 4 14.50 5.80 3 -6 -4 10.60 6.30 -3 -6 4 3.10 7.40 -3 -6 4 6.60 8.00 -3 -6 4 5.80 5.40 -3 -6 4 8.10 6.20 -3 -6 4 2.20 7.80 -3 6 4 12.00 5.00 -3 6 4 7.60 5.90 2 -6 -4 62.89 9.10 -2 -6 4 66.79 9.40 -2 -6 4 40.40 6.90 -2 -6 4 54.89 9.80 -2 -6 4 52.89 10.80 -2 -6 4 71.59 10.40 2 -6 -4 61.39 7.80 -2 6 4 76.39 7.90 -2 6 4 70.29 7.80 -1 -6 4 145.39 13.70 1 -6 -4 168.28 12.30 -1 -6 4 166.18 15.60 -1 -6 4 160.48 13.80 -1 -6 4 159.68 10.60 1 -6 -4 138.89 16.40 1 -6 -4 178.48 12.00 -1 -6 4 156.48 11.80 -1 6 4 168.38 10.40 -1 6 4 154.38 10.60 -1 6 4 173.48 13.20 -1 6 4 139.49 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4.70 -5 -1 9 7.00 5.30 -5 -1 9 9.50 5.70 -5 -1 9 5.40 4.70 -5 1 9 13.70 5.80 -5 1 9 2.30 4.40 -5 1 9 8.60 5.70 -5 1 9 2.30 4.90 -5 1 9 3.20 4.50 -4 -1 9 174.58 16.40 4 -1 -9 242.88 8.80 -4 -1 9 226.28 12.50 -4 -1 9 241.68 12.20 -4 -1 9 210.48 11.80 -4 1 9 234.78 13.20 -4 1 9 233.28 10.70 -4 1 9 234.18 12.20 -4 1 9 238.28 12.90 -4 1 9 205.68 14.80 -4 1 9 236.98 10.40 -3 -1 9 16.00 5.90 -3 -1 9 9.30 5.00 -3 -1 9 10.70 5.30 3 -1 -9 14.90 3.60 -3 1 9 15.80 5.30 -3 1 9 15.90 7.70 -3 1 9 15.60 6.00 -3 1 9 15.40 6.40 -3 1 9 8.10 5.30 -3 1 9 11.80 5.30 -2 -1 9 34.40 5.80 -2 -1 9 54.59 6.60 -2 -1 9 37.20 6.10 2 -1 -9 36.40 4.40 -2 -1 9 41.80 7.00 -2 1 9 38.80 6.70 -2 1 9 46.20 6.40 -2 1 9 41.00 7.10 -2 1 9 43.70 6.70 -2 1 9 36.40 6.10 -1 -1 9 17.70 4.40 -1 -1 9 19.60 5.00 -1 -1 9 27.00 6.00 1 -1 -9 23.60 3.80 -1 1 9 18.40 5.40 -1 1 9 19.00 5.00 -1 1 9 17.50 5.70 -1 1 9 17.80 5.10 -1 1 9 15.60 4.40 0 -1 9 10.90 4.20 0 -1 9 15.20 3.90 0 -1 9 14.60 3.90 0 -1 9 24.20 4.30 0 1 9 23.60 5.00 0 1 9 17.60 3.70 0 1 9 10.90 3.50 0 1 9 16.80 3.90 0 1 9 10.00 3.60 -7 -2 9 75.19 6.20 -7 -2 9 76.59 6.20 -7 -2 9 63.69 5.30 -7 -2 9 79.39 6.90 -7 2 9 85.59 6.20 -7 2 9 49.40 4.70 -6 -2 9 -3.60 4.50 -6 -2 9 3.70 3.90 6 -2 -9 -2.00 2.40 -6 -2 9 3.70 4.20 -6 -2 9 6.00 4.10 -6 2 9 3.10 4.20 -6 2 9 -0.20 3.40 -6 2 9 0.00 3.30 -6 2 9 -0.10 4.60 -6 2 9 -2.20 4.40 -5 -2 9 54.29 6.80 -5 -2 9 48.80 5.50 5 -2 -9 65.19 5.30 -5 -2 9 58.89 6.90 -5 2 9 70.69 7.80 -5 2 9 65.09 6.60 -5 2 9 51.09 5.60 -5 2 9 64.19 7.40 -5 2 9 68.99 7.60 -4 -2 9 84.39 9.30 4 -2 -9 99.79 6.10 -4 -2 9 78.79 8.60 -4 2 9 102.39 7.90 -4 2 9 102.49 10.40 -4 2 9 79.89 8.40 -4 2 9 102.29 9.00 -4 2 9 123.39 15.20 -4 2 9 95.59 8.00 -4 2 9 91.89 9.70 3 -2 -9 175.78 7.90 -3 2 9 190.78 11.90 -3 2 9 180.98 9.60 -3 2 9 169.18 10.60 -3 2 9 176.68 11.60 -3 2 9 191.38 10.70 2 -2 -9 48.30 4.60 -2 2 9 51.29 6.60 -2 2 9 43.10 5.60 -2 2 9 50.59 6.50 -2 2 9 65.39 8.00 -2 2 9 48.00 6.40 1 -2 -9 3.00 2.90 -1 -2 9 4.20 3.90 -1 -2 9 6.80 3.80 -1 2 9 3.20 4.30 -1 2 9 8.00 4.60 -1 2 9 3.30 5.00 -1 2 9 10.50 4.50 -1 2 9 5.10 4.40 0 -2 9 132.09 7.40 0 -2 9 175.58 9.40 0 2 9 113.99 6.50 0 2 9 132.09 6.80 0 2 9 137.49 7.30 0 2 9 121.89 6.10 0 2 9 139.29 8.10 6 -3 -9 39.80 4.80 -6 -3 9 47.60 5.20 -6 -3 9 36.80 4.20 -6 -3 9 48.10 4.80 -6 3 9 53.99 4.70 -6 3 9 33.60 4.60 -6 3 9 39.90 4.80 -6 3 9 27.40 3.90 -6 3 9 43.00 5.10 -5 -3 9 167.98 8.00 -5 -3 9 161.98 9.50 5 -3 -9 155.28 6.50 5 -3 -9 150.08 8.80 -5 3 9 152.88 10.10 -5 3 9 170.78 8.50 -5 3 9 156.88 8.10 -5 3 9 159.48 8.80 -5 3 9 153.88 9.30 4 -3 -9 82.29 5.80 -4 3 9 79.09 6.70 -4 3 9 78.09 8.20 -4 3 9 59.29 6.60 -4 3 9 84.29 6.90 3 -3 -9 33.20 4.00 -3 3 9 34.00 5.90 -3 3 9 23.80 6.90 -3 3 9 42.30 6.50 -3 3 9 33.30 5.20 -3 3 9 30.80 5.40 -3 3 9 48.70 6.70 2 -3 -9 1.60 2.80 2 -3 -9 0.00 4.00 -2 3 9 2.90 4.70 -2 3 9 2.50 4.40 -2 3 9 -2.00 4.10 -2 3 9 2.40 3.90 -2 3 9 0.40 4.30 1 -3 -9 -1.40 3.30 -1 3 9 3.10 3.90 -1 3 9 0.80 3.90 -1 3 9 -0.70 3.20 -1 3 9 3.10 3.60 -1 3 9 3.90 3.80 5 -4 -9 3.10 3.80 -5 4 9 0.90 3.60 -5 4 9 11.90 3.30 -5 4 9 -1.10 2.50 4 -4 -9 17.60 5.10 -4 4 9 11.60 3.50 -4 4 9 9.20 3.50 -4 4 9 19.10 5.10 -4 4 9 11.50 3.30 -3 4 9 17.40 4.40 -3 4 9 7.40 3.60 -3 4 9 20.50 5.30 -3 4 9 14.80 3.30 -3 4 9 15.00 3.80 2 -4 -9 0.80 2.90 -2 4 9 2.80 3.00 -2 4 9 2.80 3.10 -2 4 9 0.00 3.60 -6 0 10 1.50 3.10 -6 0 10 8.20 4.10 -5 0 10 4.40 4.50 -5 0 10 -0.50 3.10 -5 0 10 -0.50 3.40 -5 0 10 -1.30 3.80 -4 0 10 71.29 6.50 -4 0 10 78.29 6.90 -4 0 10 67.99 5.70 -3 0 10 0.20 3.30 -3 0 10 0.10 3.40 -3 0 10 -2.80 2.90 -2 0 10 642.64 15.50 -5 -1 10 113.69 7.50 -5 -1 10 105.09 6.30 -5 1 10 78.49 6.60 -5 1 10 95.89 5.90 -5 1 10 118.89 8.40 -5 1 10 90.99 7.40 -5 1 10 110.99 7.10 -4 -1 10 204.28 9.00 -4 -1 10 226.98 8.90 -4 1 10 232.48 9.50 -4 1 10 201.18 9.20 -4 1 10 226.08 8.50 -4 1 10 245.48 10.30 -3 -1 10 25.30 4.20 -3 -1 10 49.90 5.30 -3 1 10 34.60 4.40 -3 1 10 29.80 6.40 -3 1 10 34.30 4.80 -3 1 10 22.50 4.00 -3 1 10 47.30 4.90 -2 1 10 180.78 7.40 -2 1 10 206.08 7.30 -2 1 10 189.68 9.40 -5 2 10 4.50 3.70 -5 2 10 0.10 3.00 -5 2 10 2.20 3.00 -5 2 10 4.30 2.90 -4 2 10 24.30 4.30 -4 2 10 19.10 3.80 -4 2 10 24.60 3.90 -4 2 10 19.30 4.10 -3 2 10 344.07 10.20 -3 2 10 337.47 13.70 -3 2 10 353.66 11.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 76819 _shelx_res_file ; TITL berry963_a.res in P2(1)/n berry963.res created by SHELXL-2018/1 at 05:31:01 on 26-Jan-2023 REM Old TITL Berry963 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.089, Rweak 0.002, Alpha 0.016, Orientation as input REM Formula found by SHELXT: C4 N2 O CELL 1.54178 7.3685 8.0074 8.4211 90 115.741 90 ZERR 4 0.0005 0.0007 0.0009 0 0.005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 16 24 8 4 EQIV $1 -0.5+X,0.5-Y,-0.5+Z EQIV $2 1.5-X,-0.5+Y,1.5-Z L.S. 24 PLAN 1 SIZE 0.04 0.09 0.1 TEMP -173.16 CONF HTAB N1 N2_$1 HTAB N1 O1_$2 BOND $H list 4 MORE -1 fmap 2 53 acta 134 REM REM REM WGHT 0.051700 0.136600 FVAR 1.43080 O1 4 0.609845 0.633679 0.912231 11.00000 0.01560 0.02021 = 0.01771 -0.00351 0.00556 -0.00264 N1 3 0.478625 0.211599 0.512159 11.00000 0.01161 0.01849 = 0.01559 -0.00094 0.00217 -0.00032 N2 3 0.595477 0.411382 0.734391 11.00000 0.01290 0.01636 = 0.01305 0.00203 0.00363 -0.00003 C1 1 0.447583 0.335459 0.599184 11.00000 0.01343 0.01558 = 0.01298 0.00437 0.00471 -0.00126 C2 1 0.239693 0.405667 0.550862 11.00000 0.01219 0.01893 = 0.01489 0.00197 0.00396 0.00028 AFIX 23 H2A 2 0.146793 0.318525 0.555478 11.00000 -1.20000 H2B 2 0.182063 0.456487 0.431893 11.00000 -1.20000 AFIX 0 C3 1 0.282007 0.537327 0.693598 11.00000 0.01180 0.01987 = 0.01630 0.00127 0.00473 0.00049 AFIX 23 H3A 2 0.232171 0.648419 0.641205 11.00000 -1.20000 H3B 2 0.218560 0.506897 0.771872 11.00000 -1.20000 AFIX 0 C4 1 0.510483 0.535860 0.793262 11.00000 0.01418 0.01584 = 0.01256 0.00343 0.00508 0.00013 H1A 2 0.377170 0.172092 0.422119 11.00000 0.01975 H1B 2 0.602486 0.177278 0.540033 11.00000 0.02149 HKLF 4 REM berry963_a.res in P2(1)/n REM R1 = 0.0331 for 775 Fo > 4sig(Fo) and 0.0386 for all 886 data REM 72 parameters refined using 0 restraints END WGHT 0.0517 0.1366 REM Highest difference peak 0.226, deepest hole -0.180, 1-sigma level 0.043 Q1 1 0.3337 0.3637 0.5692 11.00000 0.05 0.23 ; _shelx_res_checksum 63040 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.60985(13) 0.63368(12) 0.91223(11) 0.0184(3) Uani d 1 . . N N1 0.47862(17) 0.21160(14) 0.51216(14) 0.0166(3) Uani d 1 . . N N2 0.59548(16) 0.41138(14) 0.73439(13) 0.0148(3) Uani d 1 . . C C1 0.44758(18) 0.33546(16) 0.59918(15) 0.0144(3) Uani d 1 . . C C2 0.23969(18) 0.40567(16) 0.55086(16) 0.0160(3) Uani d 1 . . H H2A 0.146793 0.318525 0.555478 0.019 Uiso calc 1 . . H H2B 0.182063 0.456487 0.431893 0.019 Uiso calc 1 . . C C3 0.28201(18) 0.53733(17) 0.69360(16) 0.0165(3) Uani d 1 . . H H3A 0.232171 0.648419 0.641205 0.020 Uiso calc 1 . . H H3B 0.218560 0.506897 0.771872 0.020 Uiso calc 1 . . C C4 0.51048(18) 0.53586(16) 0.79326(15) 0.0145(3) Uani d 1 . . H H1A 0.377(3) 0.172(2) 0.422(2) 0.020(4) Uiso d 1 . . H H1B 0.602(3) 0.177(2) 0.540(2) 0.021(4) Uiso d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0156(5) 0.0202(5) 0.0177(5) -0.0026(4) 0.0056(4) -0.0035(4) N1 0.0116(6) 0.0185(6) 0.0156(5) -0.0003(4) 0.0022(4) -0.0009(4) N2 0.0129(5) 0.0164(6) 0.0131(5) 0.0000(4) 0.0036(4) 0.0020(4) C1 0.0134(6) 0.0156(6) 0.0130(6) -0.0013(5) 0.0047(4) 0.0044(5) C2 0.0122(6) 0.0189(7) 0.0149(6) 0.0003(5) 0.0040(5) 0.0020(5) C3 0.0118(6) 0.0199(7) 0.0163(6) 0.0005(5) 0.0047(5) 0.0013(5) C4 0.0142(6) 0.0158(6) 0.0126(6) 0.0001(5) 0.0051(5) 0.0034(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N1 H1A . . 118.3(12) ? C1 N1 H1B . . 119.9(11) ? H1A N1 H1B . . 121.5(16) ? C1 N2 C4 . . 107.84(10) ? N1 C1 N2 . . 123.11(11) ? N1 C1 C2 . . 122.22(11) ? N2 C1 C2 . . 114.66(11) ? C1 C2 H2A . . 111.4 ? C1 C2 H2B . . 111.4 ? C1 C2 C3 . . 102.03(10) ? H2A C2 H2B . . 109.2 ? C3 C2 H2A . . 111.4 ? C3 C2 H2B . . 111.4 ? C2 C3 H3A . . 111.1 ? C2 C3 H3B . . 111.1 ? H3A C3 H3B . . 109.1 ? C4 C3 C2 . . 103.18(10) ? C4 C3 H3A . . 111.1 ? C4 C3 H3B . . 111.1 ? O1 C4 N2 . . 123.36(12) ? O1 C4 C3 . . 124.67(11) ? N2 C4 C3 . . 111.97(11) ? 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 C4 . 1.2313(16) ? N1 C1 . 1.3110(17) ? N1 H1A . 0.861(18) ? N1 H1B . 0.882(19) ? N2 C1 . 1.3326(16) ? N2 C4 . 1.3788(17) ? C1 C2 . 1.5122(17) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C2 C3 . 1.5257(18) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C3 C4 . 1.5204(17) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A N2 4_565 0.861(18) 2.099(19) 2.9454(16) 167.6(15) yes N1 H1B O1 2_646 0.882(19) 2.01(2) 2.8832(15) 170.9(17) 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 N1 C1 C2 C3 . . . . 177.20(11) ? N2 C1 C2 C3 . . . . -3.93(14) ? C1 N2 C4 O1 . . . . -176.49(11) ? C1 N2 C4 C3 . . . . 3.29(14) ? C1 C2 C3 C4 . . . . 5.22(12) ? C2 C3 C4 O1 . . . . 174.20(12) ? C2 C3 C4 N2 . . . . -5.57(13) ? C4 N2 C1 N1 . . . . 179.39(11) ? C4 N2 C1 C2 . . . . 0.53(14) ? _cod_database_fobs_code 2022702