#------------------------------------------------------------------------------ #$Date: 2023-03-16 04:10:54 +0100 (Thu, 16 Mar 2023) $ #$Revision: 281907 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022703.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_2022703 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_iupac 'C5 H8 N2 O' _chemical_formula_moiety 'C5 H8 N2 O' _chemical_formula_sum 'C5 H8 N2 O' _chemical_formula_weight 112.13 _chemical_name_systematic ; 6-Amino-4,5-dihydropyridin-2(3H)-one ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 84.975(13) _cell_angle_beta 71.693(13) _cell_angle_gamma 63.889(12) _cell_formula_units_Z 2 _cell_length_a 6.3296(19) _cell_length_b 7.0222(19) _cell_length_c 7.351(2) _cell_measurement_reflns_used 2665 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.744 _cell_measurement_theta_min 2.924 _cell_volume 278.05(14) _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 100.0 _diffrn_detector 'charge-coupled device (CCD) area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.962 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEXII Quazar' _diffrn_measurement_method '0.5\ \w and 0.5\ \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 9023 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 33.171 _diffrn_reflns_theta_min 2.924 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_correction_T_min 0.9292 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2016) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 120 _exptl_crystal_size_max 0.161 _exptl_crystal_size_mid 0.051 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.442 _refine_diff_density_min -0.267 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 79 _refine_ls_number_reflns 2048 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0426 _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^)+(0.0544P)^2^+0.1043P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.1195 _reflns_number_gt 1680 _reflns_number_total 2048 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ep3031sup1.cif _cod_data_source_block 4 _cod_original_cell_volume 278.06(14) _cod_database_code 2022703 _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 0.985 _shelx_estimated_absorpt_t_max 0.999 _shelx_hkl_file ; 1 2 0 49.60 2.40 1 2 0 49.90 2.20 -1 -2 0 50.39 2.30 -1 -2 0 50.19 2.10 -1 -2 0 49.20 1.90 -1 -2 0 51.19 1.80 2 4 0 1.60 0.70 2 4 0 0.40 0.80 -2 -4 0 1.90 0.90 -2 -4 0 1.00 0.40 -2 -4 0 0.20 0.50 -2 -4 0 0.00 0.50 3 6 0 246.88 9.60 3 6 0 247.98 10.30 -3 -6 0 229.68 9.70 -3 -6 0 247.88 8.70 -3 -6 0 245.78 9.20 4 8 0 58.79 4.10 4 8 0 55.19 5.00 -4 -8 0 50.69 4.70 -4 -8 0 56.19 3.20 5 10 0 -0.30 2.20 5 10 0 0.10 2.70 -5 -10 0 1.40 2.20 -5 -10 -1 -1.00 1.40 -5 -10 -1 -0.60 2.20 5 10 1 -0.10 2.60 5 10 1 1.80 2.40 -4 -8 -1 52.39 4.70 -4 -8 -1 70.49 3.40 4 8 1 65.59 4.80 4 8 1 64.59 4.50 -3 -6 -1 405.66 15.30 -3 -6 -1 405.26 14.10 -3 -6 -1 417.16 14.90 3 6 1 417.06 15.60 3 6 1 422.16 15.10 -2 -4 -1 7.90 1.10 -2 -4 -1 9.60 1.20 -2 -4 -1 8.20 0.50 -2 -4 -1 8.20 0.70 -2 -4 -1 6.60 1.20 2 4 1 11.60 1.50 2 4 1 7.70 1.10 -1 -2 -1 382.36 12.80 -1 -2 -1 382.06 13.00 -1 -2 -1 396.56 13.00 1 2 1 383.76 13.10 1 2 1 376.86 13.00 0 0 -1 597.84 19.30 0 0 -1 581.44 19.50 0 0 -1 608.34 19.50 0 0 -1 591.94 19.30 0 0 1 591.44 19.40 0 0 1 586.64 19.40 0 0 1 602.54 19.30 0 0 1 576.94 19.30 1 2 -1 70.29 2.80 1 2 -1 66.49 2.80 1 2 -1 67.99 2.50 1 2 -1 72.69 3.20 -1 -2 1 68.49 2.60 -1 -2 1 70.59 2.60 -1 -2 1 66.39 2.90 -1 -2 1 68.69 2.70 2 4 -1 0.10 1.00 2 4 -1 1.30 0.70 -2 -4 1 1.50 0.80 -2 -4 1 1.20 0.50 -2 -4 1 2.70 0.60 -2 -4 1 1.60 0.50 3 6 -1 1050.29 36.60 3 6 -1 1018.40 35.80 -3 -6 1 1048.00 35.10 -3 -6 1 1066.99 34.90 -3 -6 1 1061.29 36.00 4 8 -1 34.80 4.30 4 8 -1 45.80 4.00 -4 -8 1 36.40 3.70 -4 -8 1 44.40 3.10 5 10 -1 3.00 3.00 5 10 -1 4.40 2.60 -5 -10 1 3.60 2.70 -5 -10 -2 0.50 2.20 -5 -10 -2 -0.90 1.40 5 10 2 1.50 2.30 5 10 2 -0.40 2.40 -4 -8 -2 2.60 1.70 -4 -8 -2 0.40 1.20 -4 -8 -2 2.70 1.10 4 8 2 2.50 1.70 4 8 2 2.20 1.60 -3 -6 -2 80.29 3.30 -3 -6 -2 79.39 4.20 -3 -6 -2 81.19 4.40 3 6 2 76.59 4.20 3 6 2 79.99 4.50 -2 -4 -2 69.19 3.10 -2 -4 -2 73.99 2.70 -2 -4 -2 75.69 3.60 -2 -4 -2 78.59 3.60 2 4 2 78.29 3.70 2 4 2 77.79 3.50 -1 -2 -2 248.08 8.70 -1 -2 -2 253.17 8.30 -1 -2 -2 267.37 8.90 -1 -2 -2 259.37 9.00 -1 -2 -2 240.78 8.80 1 2 2 254.37 8.80 1 2 2 248.58 8.70 1 2 2 255.27 8.90 1 2 2 250.27 8.40 0 0 -2 3036.90 98.49 0 0 -2 3036.10 98.19 0 0 -2 2956.60 98.49 0 0 2 2966.40 98.29 0 0 2 3108.49 98.39 0 0 2 3056.19 98.39 0 0 2 3040.90 98.29 0 0 2 2994.90 98.09 1 2 -2 439.36 15.00 1 2 -2 422.06 14.70 1 2 -2 442.96 15.40 1 2 -2 433.56 14.50 -1 -2 2 450.15 15.00 -1 -2 2 430.56 14.80 -1 -2 2 435.36 14.50 2 4 -2 0.30 1.10 2 4 -2 2.30 0.80 2 4 -2 0.50 0.80 -2 -4 2 0.60 0.80 -2 -4 2 1.70 0.70 -2 -4 2 1.80 0.70 -2 -4 2 0.50 0.40 3 6 -2 3.80 1.30 3 6 -2 1.50 1.50 -3 -6 2 2.90 1.40 -3 -6 2 3.00 1.10 -3 -6 2 3.10 1.00 4 8 -2 2.30 1.60 4 8 -2 0.00 1.90 -4 -8 2 2.10 1.50 -4 -8 2 3.90 1.90 -5 -10 2 3.80 2.80 -5 -10 -3 29.10 3.80 -5 -10 -3 21.80 3.80 -5 -10 -3 25.40 2.60 5 10 3 30.20 4.30 5 10 3 27.20 4.00 -4 -8 -3 4.00 1.10 -4 -8 -3 3.70 1.90 -4 -8 -3 5.40 1.70 -4 -8 -3 6.80 1.80 4 8 3 2.50 1.80 4 8 3 3.90 1.70 -3 -6 -3 1.30 1.10 -3 -6 -3 1.60 1.20 -3 -6 -3 1.80 1.00 3 6 3 3.20 1.20 3 6 3 0.40 1.00 -2 -4 -3 4.70 1.10 -2 -4 -3 3.60 1.00 -2 -4 -3 5.90 1.20 2 4 3 3.80 0.90 2 4 3 4.10 1.10 2 4 3 4.10 0.40 -1 -2 -3 26.50 1.10 -1 -2 -3 26.40 1.80 -1 -2 -3 23.70 1.60 -1 -2 -3 26.30 1.70 1 2 3 24.40 1.30 1 2 3 26.10 1.60 1 2 3 24.00 1.30 1 2 3 26.30 1.60 0 0 -3 121.69 4.50 0 0 -3 118.89 4.90 0 0 -3 124.09 5.00 0 0 3 120.79 4.70 0 0 3 122.09 4.60 0 0 3 125.49 4.20 0 0 3 127.39 4.30 0 0 3 123.69 4.80 1 2 -3 206.18 8.00 1 2 -3 200.98 7.20 1 2 -3 190.78 7.10 1 2 -3 209.18 7.70 -1 -2 3 201.58 7.40 -1 -2 3 199.98 7.00 -1 -2 3 196.68 7.00 -1 -2 3 194.78 7.60 2 4 -3 92.69 4.00 2 4 -3 86.59 4.90 -2 -4 3 80.99 4.30 -2 -4 3 85.59 3.70 -2 -4 3 85.29 3.40 -2 -4 3 85.79 3.90 3 6 -3 134.09 7.30 3 6 -3 129.99 6.20 -3 -6 3 134.09 5.60 -3 -6 3 129.79 5.80 -3 -6 3 141.39 6.60 4 8 -3 70.59 4.90 4 8 -3 68.19 6.40 -4 -8 3 68.89 5.00 -4 -8 3 73.49 4.30 -5 -10 -4 84.69 6.70 -5 -10 -4 83.19 4.60 -5 -10 -4 81.49 7.00 5 10 4 92.79 6.60 5 10 4 82.89 6.40 -4 -8 -4 0.90 1.50 -4 -8 -4 2.80 2.00 -4 -8 -4 0.30 1.60 -4 -8 -4 1.60 1.00 4 8 4 0.40 1.50 4 8 4 0.40 1.50 -3 -6 -4 25.40 2.80 -3 -6 -4 22.30 2.70 -3 -6 -4 25.70 2.70 -3 -6 -4 22.80 1.50 3 6 4 23.00 2.30 3 6 4 25.50 2.60 -2 -4 -4 236.08 9.40 -2 -4 -4 243.88 8.20 -2 -4 -4 240.38 9.20 -2 -4 -4 232.48 9.20 2 4 4 237.88 9.20 2 4 4 241.28 8.80 2 4 4 242.28 8.60 -1 -2 -4 20.70 1.80 -1 -2 -4 15.70 1.70 -1 -2 -4 16.40 1.10 -1 -2 -4 13.70 1.60 1 2 4 19.60 1.40 1 2 4 17.30 1.10 1 2 4 16.90 1.60 0 0 -4 4.60 1.10 0 0 -4 5.30 0.90 0 0 -4 4.30 1.10 0 0 -4 4.80 0.80 0 0 4 3.90 0.50 0 0 4 5.50 0.90 0 0 4 3.60 0.70 0 0 4 3.10 0.50 0 0 4 5.70 1.00 1 2 -4 46.90 3.00 1 2 -4 56.79 2.60 1 2 -4 54.19 3.40 1 2 -4 53.99 2.40 -1 -2 4 56.19 2.90 -1 -2 4 53.39 3.10 -1 -2 4 55.19 2.40 -1 -2 4 46.30 2.40 2 4 -4 31.80 3.50 2 4 -4 27.90 2.30 -2 -4 4 28.40 3.00 -2 -4 4 28.10 2.20 -2 -4 4 32.00 2.60 3 6 -4 5.00 1.50 3 6 -4 2.40 2.10 -3 -6 4 2.80 1.70 -3 -6 4 3.40 1.20 -3 -6 4 3.20 1.20 4 8 -4 4.60 2.90 4 8 -4 4.70 2.10 -4 -8 4 8.40 2.00 -5 -10 -5 1.00 2.70 5 10 5 5.90 3.40 -4 -8 -5 -2.00 1.50 -4 -8 -5 1.70 2.00 -4 -8 -5 -0.60 1.00 -4 -8 -5 -0.40 1.60 4 8 5 0.40 1.60 4 8 5 -1.70 1.40 -3 -6 -5 15.10 2.30 -3 -6 -5 16.60 1.50 -3 -6 -5 17.60 2.60 -3 -6 -5 14.40 2.20 3 6 5 14.70 2.00 3 6 5 15.50 2.20 -2 -4 -5 256.87 10.40 -2 -4 -5 255.47 10.30 -2 -4 -5 260.77 9.10 -2 -4 -5 269.27 10.30 2 4 5 258.57 9.40 -1 -2 -5 1.50 0.80 -1 -2 -5 0.50 0.90 -1 -2 -5 0.30 0.90 -1 -2 -5 0.80 0.60 1 2 5 1.60 0.70 1 2 5 1.20 0.70 1 2 5 0.60 0.50 0 0 -5 35.20 3.00 0 0 -5 40.60 2.80 0 0 -5 45.00 2.60 0 0 -5 44.00 2.30 0 0 5 42.60 2.30 0 0 5 40.50 2.50 1 2 -5 208.48 8.40 1 2 -5 208.18 8.80 1 2 -5 186.88 7.40 1 2 -5 201.18 7.30 -1 -2 5 199.08 7.30 -1 -2 5 203.08 8.00 -1 -2 5 200.68 7.40 2 4 -5 7.60 2.20 2 4 -5 14.60 1.70 -2 -4 5 10.60 1.70 -2 -4 5 11.00 2.20 -2 -4 5 11.20 1.50 3 6 -5 3.30 2.30 3 6 -5 -0.70 1.20 -3 -6 5 1.40 1.30 -3 -6 5 -1.10 1.30 4 8 -5 11.10 4.00 -4 -8 5 5.50 2.20 -4 -8 -6 0.50 1.90 -4 -8 -6 -2.60 1.80 -4 -8 -6 0.00 1.20 -4 -8 -6 -0.60 2.10 4 8 6 -2.50 1.50 -3 -6 -6 6.20 2.00 -3 -6 -6 13.70 2.60 -3 -6 -6 12.90 1.40 -3 -6 -6 13.40 2.40 -2 -4 -6 35.10 3.20 -2 -4 -6 25.20 2.80 -2 -4 -6 24.10 2.80 -2 -4 -6 30.30 1.90 -1 -2 -6 16.90 2.30 -1 -2 -6 12.40 1.90 -1 -2 -6 13.20 1.50 -1 -2 -6 16.70 2.20 1 2 6 16.20 1.70 1 2 6 16.90 1.80 0 0 -6 56.49 2.90 0 0 -6 55.09 3.20 0 0 -6 53.09 3.50 0 0 6 43.60 2.70 0 0 6 51.19 3.00 1 2 -6 209.28 8.00 1 2 -6 210.88 8.90 1 2 -6 202.88 7.80 1 2 -6 207.78 9.40 -1 -2 6 195.68 7.70 -1 -2 6 200.08 8.30 2 4 -6 2.40 1.90 -2 -4 6 4.00 1.40 3 6 -6 2.80 2.80 -3 -6 6 1.90 1.50 -4 -8 -7 10.80 3.20 -4 -8 -7 8.90 1.90 -4 -8 -7 9.10 2.70 -4 -8 -7 18.30 3.60 -3 -6 -7 90.19 4.30 -3 -6 -7 97.69 5.90 -3 -6 -7 94.39 5.90 -3 -6 -7 92.39 5.90 -2 -4 -7 132.99 5.50 -2 -4 -7 132.99 6.60 -2 -4 -7 134.09 6.90 -2 -4 -7 125.79 6.80 -1 -2 -7 4.10 1.50 -1 -2 -7 4.60 1.90 -1 -2 -7 4.20 1.60 -1 -2 -7 6.00 1.30 1 2 7 4.80 1.40 1 2 7 3.70 1.20 0 0 -7 20.20 2.70 0 0 -7 17.70 2.40 0 0 -7 21.30 2.00 1 2 -7 45.10 3.00 1 2 -7 47.10 4.60 -1 -2 7 47.70 3.80 2 4 -7 4.10 2.50 -2 -4 7 4.50 1.70 3 6 -7 1.10 3.20 -3 -6 7 -1.60 1.70 -3 -6 -8 -2.80 1.80 -3 -6 -8 -2.00 1.90 -3 -6 -8 -2.10 1.30 -3 -6 -8 0.20 2.00 -2 -4 -8 183.48 8.50 -2 -4 -8 175.08 8.60 -2 -4 -8 169.98 8.80 -2 -4 -8 173.48 7.30 -1 -2 -8 34.00 3.70 -1 -2 -8 34.90 3.50 -1 -2 -8 26.40 3.50 -1 -2 -8 38.60 3.10 1 2 8 32.50 3.00 1 2 8 41.40 3.40 0 0 -8 70.49 4.90 0 0 -8 66.39 4.20 0 0 -8 59.69 5.30 0 0 -8 64.99 3.90 0 0 8 68.89 4.30 0 0 8 65.69 3.80 1 2 -8 177.18 9.50 -1 -2 8 171.08 8.10 2 4 -8 19.20 3.90 -2 -4 8 11.70 2.60 -3 -6 -9 52.39 5.50 -3 -6 -9 72.39 6.60 -3 -6 -9 62.59 6.10 -3 -6 -9 71.89 4.50 -2 -4 -9 3.50 2.20 -2 -4 -9 0.80 2.00 -2 -4 -9 1.40 1.70 -2 -4 -9 2.60 2.50 -1 -2 -9 -1.10 2.10 -1 -2 -9 -0.10 1.70 -1 -2 -9 1.20 2.00 -1 -2 -9 0.30 1.60 1 2 9 1.20 1.50 0 0 -9 6.60 2.80 0 0 -9 11.40 2.30 0 0 9 7.50 2.10 1 2 -9 107.39 7.60 -1 -2 9 86.99 5.80 2 4 -9 2.60 3.70 -2 -4 9 -0.30 2.30 -2 -4 -10 3.80 2.90 -2 -4 -10 8.40 3.60 -2 -4 -10 12.00 2.90 -2 -4 -10 8.00 2.80 -1 -2 -10 0.00 2.40 -1 -2 -10 1.70 2.20 -1 -2 -10 2.50 2.40 -1 -2 -10 0.80 2.80 0 0 -10 13.80 4.10 0 0 -10 14.60 2.80 0 0 10 19.10 3.30 0 -1 10 126.59 7.30 0 1 -10 142.99 9.30 1 1 10 18.00 2.90 1 1 10 15.70 2.70 -1 -1 -10 21.50 4.00 -1 -1 -10 20.20 3.30 -1 -1 -10 11.30 3.30 -1 -1 -10 10.70 2.60 -2 -3 -10 15.50 3.50 -2 -3 -10 11.00 3.10 -2 -3 -10 11.80 2.60 -2 -3 -10 11.40 3.60 -3 -5 -10 44.50 7.60 -3 -5 -10 48.90 5.80 -1 -3 9 22.00 3.20 1 3 -9 12.90 3.90 0 -1 9 -1.00 1.50 0 1 -9 2.50 2.50 0 1 -9 0.80 1.70 1 1 9 7.10 2.00 1 1 9 3.00 1.50 -1 -1 -9 7.20 1.90 -1 -1 -9 -0.60 1.50 -1 -1 -9 5.20 2.20 -1 -1 -9 -0.20 1.80 -2 -3 -9 17.80 2.40 -2 -3 -9 23.60 3.50 -2 -3 -9 21.90 3.20 -2 -3 -9 22.60 3.50 -3 -5 -9 83.39 4.60 -3 -5 -9 65.89 5.80 -3 -5 -9 81.29 6.60 -3 -5 -9 98.69 6.90 -2 -5 8 10.10 2.50 2 5 -8 13.80 3.90 -1 -3 8 18.10 2.60 1 3 -8 14.60 3.40 0 -1 8 114.99 5.80 0 -1 8 109.39 5.30 0 1 -8 105.59 6.80 0 1 -8 112.79 5.60 0 1 -8 112.19 5.30 0 1 -8 108.99 6.40 1 1 8 142.39 6.40 1 1 8 129.79 6.20 -1 -1 -8 132.99 5.90 -1 -1 -8 153.98 7.60 -1 -1 -8 131.89 6.70 -1 -1 -8 134.39 7.00 2 3 8 36.30 3.30 2 3 8 32.10 3.60 -2 -3 -8 30.20 3.50 -2 -3 -8 24.70 3.40 -2 -3 -8 39.80 3.80 -2 -3 -8 43.00 3.00 -3 -5 -8 8.80 1.60 -3 -5 -8 10.60 2.60 -3 -5 -8 1.90 1.80 -3 -5 -8 1.70 1.90 -4 -7 -8 7.70 2.70 -4 -7 -8 3.20 2.40 -4 -7 -8 2.20 1.60 -4 -7 -8 5.30 2.70 -3 -7 7 9.10 2.60 3 7 -7 4.00 3.80 -2 -5 7 59.89 4.20 2 5 -7 48.80 5.50 -1 -3 7 55.29 3.80 1 3 -7 52.79 3.20 1 3 -7 56.09 5.10 0 -1 7 20.40 2.10 0 -1 7 21.30 2.40 0 1 -7 25.60 3.00 0 1 -7 17.40 2.80 0 1 -7 23.10 2.10 0 1 -7 17.50 2.10 1 1 7 5.90 1.40 1 1 7 6.10 1.40 -1 -1 -7 5.30 1.50 -1 -1 -7 6.60 1.60 -1 -1 -7 5.50 1.30 -1 -1 -7 7.10 1.80 2 3 7 98.29 4.90 2 3 7 86.09 4.30 -2 -3 -7 89.59 5.00 -2 -3 -7 97.19 5.40 -2 -3 -7 93.19 5.20 -2 -3 -7 103.69 4.20 -3 -5 -7 93.69 4.10 -3 -5 -7 89.69 5.30 -3 -5 -7 95.19 5.70 -3 -5 -7 94.49 5.60 -4 -7 -7 91.89 6.30 -4 -7 -7 99.59 6.30 -4 -7 -7 105.19 6.50 -4 -7 -7 102.69 4.60 -3 -7 6 0.70 1.60 3 7 -6 -1.30 2.80 -2 -5 6 58.79 3.90 2 5 -6 60.19 5.60 -1 -3 6 6.10 1.40 1 3 -6 4.90 2.00 1 3 -6 7.60 1.30 0 -1 6 57.69 3.00 0 -1 6 55.39 3.30 0 1 -6 56.49 3.00 0 1 -6 58.99 3.90 0 1 -6 53.09 3.60 1 1 6 216.58 8.30 1 1 6 220.98 8.50 -1 -1 -6 212.48 8.70 -1 -1 -6 214.88 8.00 -1 -1 -6 211.78 8.80 -1 -1 -6 235.08 9.20 2 3 6 41.30 2.70 2 3 6 39.60 2.30 -2 -3 -6 40.90 2.90 -2 -3 -6 45.10 2.20 -2 -3 -6 44.80 3.70 -2 -3 -6 38.10 3.30 -3 -5 -6 30.90 1.80 -3 -5 -6 34.30 3.20 -3 -5 -6 29.80 3.20 -3 -5 -6 29.40 3.10 4 7 6 -0.20 1.40 -4 -7 -6 -2.50 1.40 -4 -7 -6 0.00 0.80 -4 -7 -6 0.20 1.60 -4 -7 -6 -0.50 1.50 5 9 6 44.60 4.60 -5 -9 -6 36.80 4.60 -5 -9 -6 40.20 3.10 -5 -9 -6 42.90 4.80 -5 -9 -6 33.10 4.40 -3 -7 5 7.00 2.00 -3 -7 5 6.70 1.80 3 7 -5 4.40 1.80 3 7 -5 5.40 3.00 -2 -5 5 29.70 2.30 -2 -5 5 25.60 2.50 2 5 -5 23.50 3.40 2 5 -5 26.70 2.50 -1 -3 5 8.30 1.10 -1 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2.30 7 5 -4 16.90 3.10 7 5 -4 10.50 4.40 -7 -5 4 12.40 3.20 -7 -5 4 11.60 2.50 -7 -5 4 14.10 3.10 -7 -5 4 13.10 3.00 1 -7 -5 1.50 2.50 -1 7 5 1.40 2.70 2 -5 -5 239.08 11.00 -2 5 5 254.87 10.90 3 -3 -5 16.80 3.30 -3 3 5 12.80 2.40 4 -1 -5 14.40 3.80 -4 1 5 11.50 2.30 -4 1 5 14.20 2.40 5 1 -5 0.10 2.50 -5 -1 5 2.50 1.50 -5 -1 5 1.00 1.80 -5 -1 5 3.50 1.90 6 3 -5 -1.70 2.70 -6 -3 5 -0.10 2.00 -6 -3 5 0.70 1.70 2 -5 -6 5.70 2.50 -4 1 6 1.30 2.10 5 1 -6 175.08 10.20 -5 -1 6 176.08 8.80 6 3 -6 26.60 5.30 -4 1 7 4.40 2.70 5 1 -7 1.80 4.30 4 -2 10 2.20 2.20 4 -2 10 1.90 2.40 -4 2 -10 7.00 2.80 -4 2 -10 2.10 2.20 5 0 10 63.09 5.40 5 0 10 59.29 5.00 -5 0 -10 68.49 4.40 -5 0 -10 66.59 5.50 6 2 10 5.90 2.40 6 2 10 4.00 2.20 -6 -2 -10 8.70 2.50 -6 -2 -10 5.80 1.80 -6 -2 -10 8.20 3.00 3 -4 9 2.40 2.00 3 -4 9 -1.30 2.10 -3 4 -9 -1.50 2.00 -3 4 -9 0.10 2.50 4 -2 9 3.20 1.90 4 -2 9 0.40 1.80 -4 2 -9 -1.10 1.90 -4 2 -9 -0.40 1.70 5 0 9 24.50 3.10 5 0 9 16.10 2.70 -5 0 -9 21.80 2.40 -5 0 -9 20.90 3.00 6 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1.20 -3 4 -4 1.70 1.20 -3 4 -4 0.10 1.00 4 -2 4 21.00 2.10 4 -2 4 25.70 2.60 -4 2 -4 18.00 1.90 -4 2 -4 17.50 2.00 -4 2 -4 23.10 1.80 5 0 4 127.49 5.60 5 0 4 114.99 5.60 -5 0 -4 136.79 5.70 -5 0 -4 122.29 5.10 6 2 4 218.28 8.70 6 2 4 225.38 8.70 6 2 4 228.68 8.80 -6 -2 -4 215.08 8.80 -6 -2 -4 217.28 8.90 7 4 4 7.10 1.70 7 4 4 7.20 1.50 -7 -4 -4 11.20 2.00 -7 -4 -4 8.90 1.60 8 6 4 0.10 1.50 8 6 4 -0.90 1.90 -8 -6 -4 -1.20 1.50 -8 -6 -4 0.90 1.10 9 8 4 29.80 4.60 -9 -8 -4 23.10 3.40 1 -8 3 7.80 2.40 -1 8 -3 8.80 2.60 2 -6 3 56.29 4.50 -2 6 -3 55.99 4.60 -2 6 -3 58.49 3.60 3 -4 3 476.55 16.80 3 -4 3 462.85 17.40 -3 4 -3 481.05 16.60 -3 4 -3 473.65 17.30 -3 4 -3 474.55 17.40 4 -2 3 44.40 2.70 4 -2 3 40.90 3.30 -4 2 -3 38.90 2.80 -4 2 -3 39.90 2.20 -4 2 -3 40.10 2.60 5 0 3 2.90 1.10 5 0 3 1.80 0.90 -5 0 -3 2.60 1.10 -5 0 -3 3.50 0.90 -5 0 -3 2.50 1.00 -5 0 -3 3.40 0.60 6 2 3 29.30 2.50 6 2 3 24.90 2.20 6 2 3 15.40 2.00 -6 -2 -3 23.50 2.40 -6 -2 -3 24.00 1.50 -6 -2 -3 18.80 2.20 7 4 3 76.49 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4.70 -3 4 -1 90.69 4.10 -3 4 -1 82.69 4.80 -3 4 -1 85.39 4.10 4 -2 1 27.90 2.60 4 -2 1 31.00 2.50 -4 2 -1 34.80 2.40 -4 2 -1 28.60 2.00 -4 2 -1 33.60 3.00 -4 2 -1 31.50 2.60 5 0 1 2.70 1.00 5 0 1 4.60 1.10 -5 0 -1 3.40 1.20 -5 0 -1 2.10 0.90 -5 0 -1 3.50 1.10 -5 0 -1 3.40 0.80 6 2 1 77.29 4.20 -6 -2 -1 66.69 3.50 -6 -2 -1 74.69 4.30 -6 -2 -1 75.79 4.00 7 4 1 86.29 5.10 7 4 1 90.29 5.30 -7 -4 -1 95.89 5.40 -7 -4 -1 91.39 4.80 -7 -4 -1 85.69 4.30 8 6 1 17.50 3.00 8 6 1 12.30 3.10 -8 -6 -1 8.70 1.80 -8 -6 -1 7.30 2.20 -8 -6 -1 15.80 2.40 1 -8 0 2.20 1.90 -1 8 0 2.00 2.10 2 -6 0 0.50 1.40 -2 6 0 1.10 1.50 3 -4 0 92.59 5.00 3 -4 0 89.19 4.20 -3 4 0 93.29 4.30 -3 4 0 98.09 4.20 -3 4 0 87.69 5.10 -3 4 0 93.29 4.90 4 -2 0 94.49 4.60 4 -2 0 88.29 4.20 -4 2 0 88.69 4.00 -4 2 0 90.69 4.40 -4 2 0 87.59 4.80 -4 2 0 95.99 4.60 5 0 0 107.19 4.60 -5 0 0 100.89 5.30 -5 0 0 115.99 4.40 -5 0 0 105.19 4.90 -5 0 0 100.39 5.00 6 2 0 61.39 3.70 -6 -2 0 59.59 2.60 -6 -2 0 53.59 3.70 -6 -2 0 54.69 3.50 -6 -2 0 62.69 3.40 7 4 0 -1.10 1.60 7 4 0 0.40 1.30 -7 -4 0 -0.70 1.20 -7 -4 0 0.40 1.20 -7 -4 0 0.90 0.70 -7 -4 0 -0.10 1.10 8 6 0 -0.70 2.50 8 6 0 0.20 1.90 -8 -6 0 1.70 1.70 -8 -6 0 -0.50 1.00 -8 -6 0 0.10 1.60 -8 -6 0 1.10 1.90 1 -8 -1 43.70 4.40 -1 8 1 73.09 5.80 2 -6 -1 12.90 2.40 -2 6 1 9.60 2.40 3 -4 -1 79.59 4.60 -3 4 1 89.19 4.60 -3 4 1 75.39 4.70 -3 4 1 80.99 3.90 -3 4 1 83.99 4.00 4 -2 -1 3.20 1.20 -4 2 1 0.70 1.00 -4 2 1 1.50 1.10 -4 2 1 2.70 1.30 -4 2 1 1.80 0.90 -5 0 1 0.40 1.00 -5 0 1 1.20 0.80 -5 0 1 -0.20 1.00 -5 0 1 0.80 1.10 6 2 -1 33.80 3.10 -6 -2 1 42.40 3.80 -6 -2 1 34.60 3.10 -6 -2 1 31.70 3.00 -6 -2 1 35.80 2.20 7 4 -1 43.80 4.40 7 4 -1 52.09 4.30 -7 -4 1 43.70 2.60 -7 -4 1 41.10 3.70 -7 -4 1 41.90 4.10 -7 -4 1 48.80 3.50 8 6 -1 48.60 5.80 8 6 -1 59.39 5.20 -8 -6 1 29.90 3.60 -8 -6 1 34.80 3.80 -8 -6 1 58.19 3.30 -8 -6 1 54.09 5.10 1 -8 -2 24.40 3.60 -1 8 2 24.40 3.90 2 -6 -2 0.80 1.70 -2 6 2 -1.50 1.60 3 -4 -2 36.40 3.30 -3 4 2 33.10 3.40 -3 4 2 25.60 2.30 4 -2 -2 96.79 4.70 -4 2 2 92.99 4.20 -4 2 2 85.99 4.90 -4 2 2 92.89 4.60 -4 2 2 85.69 5.00 -5 0 2 33.00 3.00 -5 0 2 32.50 2.40 -5 0 2 24.10 2.80 -5 0 2 32.40 3.10 -6 -2 2 78.49 3.70 -6 -2 2 69.59 4.70 -6 -2 2 74.99 4.50 -6 -2 2 75.99 4.60 7 4 -2 1.20 1.60 7 4 -2 2.10 2.60 -7 -4 2 1.90 1.70 -7 -4 2 2.60 1.70 -7 -4 2 0.00 1.50 -7 -4 2 1.70 1.20 8 6 -2 -1.70 2.10 8 6 -2 -0.80 3.40 -8 -6 2 -1.40 2.00 -8 -6 2 0.80 1.80 -8 -6 2 -0.10 2.20 -8 -6 2 -3.70 1.90 1 -8 -3 1.80 2.40 -1 8 3 1.50 2.80 2 -6 -3 -0.80 1.70 -2 6 3 -3.00 1.70 3 -4 -3 72.19 4.60 -3 4 3 64.19 4.50 4 -2 -3 46.10 3.20 -4 2 3 38.30 3.30 -4 2 3 51.79 4.00 -4 2 3 44.40 2.80 -4 2 3 49.00 3.70 -5 0 3 6.80 1.50 -5 0 3 10.70 2.00 -5 0 3 6.80 1.80 -5 0 3 9.30 2.00 -6 -2 3 13.30 1.80 -6 -2 3 8.20 2.10 -6 -2 3 4.70 1.90 -6 -2 3 11.10 2.40 7 4 -3 40.70 5.10 7 4 -3 29.80 3.50 -7 -4 3 35.70 3.90 -7 -4 3 43.10 3.20 -7 -4 3 29.40 3.70 -7 -4 3 27.10 3.40 -1 8 4 -0.60 3.00 2 -6 -4 14.10 3.00 -2 6 4 12.50 3.10 3 -4 -4 10.10 2.40 -3 4 4 7.10 2.20 -4 2 4 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2.30 3 -5 8 0.60 2.10 -3 5 -8 5.00 2.30 4 -3 8 46.40 4.20 4 -3 8 53.39 4.80 -4 3 -8 59.79 5.00 -4 3 -8 57.39 4.00 5 -1 8 8.60 2.20 5 -1 8 6.80 2.00 -5 1 -8 7.10 1.60 -5 1 -8 8.70 2.10 6 1 8 0.00 1.40 6 1 8 -0.40 1.40 -6 -1 -8 -0.20 1.20 7 3 8 -1.90 1.50 7 3 8 -1.50 1.50 -7 -3 -8 0.00 1.00 -7 -3 -8 0.50 2.00 8 5 8 11.00 2.70 -8 -5 -8 11.60 3.20 3 -5 7 1.20 1.80 3 -5 7 1.80 1.70 -3 5 -7 1.60 1.80 4 -3 7 55.29 4.60 4 -3 7 61.69 4.70 -4 3 -7 64.39 4.40 -4 3 -7 62.29 3.70 5 -1 7 17.10 2.40 5 -1 7 18.10 2.70 -5 1 -7 23.90 2.20 -5 1 -7 17.80 2.30 6 1 7 5.50 1.70 6 1 7 3.40 1.70 -6 -1 -7 3.30 1.20 7 3 7 87.69 5.20 7 3 7 88.89 4.90 -7 -3 -7 83.99 3.70 8 5 7 3.30 1.90 -8 -5 -7 1.30 2.00 2 -7 6 51.09 4.90 3 -5 6 1.90 1.70 3 -5 6 2.50 1.60 -3 5 -6 2.70 1.90 -3 5 -6 3.50 1.70 4 -3 6 1.40 1.30 4 -3 6 1.70 1.50 -4 3 -6 1.70 1.20 -4 3 -6 1.50 1.40 5 -1 6 4.40 1.40 5 -1 6 4.60 1.60 -5 1 -6 3.70 1.10 -5 1 -6 3.10 1.20 6 1 6 10.00 2.00 6 1 6 8.90 1.70 -6 -1 -6 9.30 1.40 7 3 6 114.49 5.70 7 3 6 102.99 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4 -7 10.20 2.50 -4 4 -7 14.20 2.30 5 -2 7 19.90 2.70 5 -2 7 15.10 2.50 -5 2 -7 9.60 2.10 -5 2 -7 16.20 2.00 6 0 7 41.10 4.00 6 0 7 43.00 3.60 -6 0 -7 38.30 2.60 -6 0 -7 29.60 2.80 7 2 7 12.00 2.40 7 2 7 8.10 2.00 -7 -2 -7 8.30 1.50 8 4 7 7.90 2.30 8 4 7 7.00 1.90 -8 -4 -7 4.10 2.10 -8 -4 -7 7.50 2.10 3 -6 6 2.40 2.10 -3 6 -6 2.10 2.00 4 -4 6 -0.40 1.30 4 -4 6 -2.70 1.30 -4 4 -6 0.60 1.60 -4 4 -6 -0.10 1.40 5 -2 6 43.80 3.90 5 -2 6 53.29 3.60 -5 2 -6 50.39 3.60 -5 2 -6 50.19 3.00 6 0 6 66.59 4.40 6 0 6 66.09 4.10 -6 0 -6 61.19 3.60 -6 0 -6 66.69 3.10 7 2 6 39.60 3.40 7 2 6 49.60 4.00 -7 -2 -6 40.00 2.40 8 4 6 10.10 2.00 -8 -4 -6 7.50 1.90 3 -6 5 7.80 2.30 -3 6 -5 14.50 2.90 -3 6 -5 13.60 2.40 4 -4 5 179.18 7.80 4 -4 5 183.28 8.50 -4 4 -5 191.88 7.60 -4 4 -5 184.68 8.50 -4 4 -5 178.18 8.20 5 -2 5 14.80 2.40 5 -2 5 13.40 2.00 -5 2 -5 12.40 2.00 -5 2 -5 13.10 1.70 -5 2 -5 8.90 1.70 6 0 5 0.20 1.20 6 0 5 1.90 1.30 -6 0 -5 0.10 1.00 -6 0 -5 0.60 0.80 -6 0 -5 1.10 0.90 7 2 5 34.30 3.00 7 2 5 31.80 3.10 -7 -2 -5 26.80 2.90 -7 -2 -5 30.80 3.00 -7 -2 -5 27.90 1.80 8 4 5 105.69 5.70 8 4 5 105.99 5.50 -8 -4 -5 113.99 6.00 -8 -4 -5 106.89 5.70 9 6 5 18.70 3.20 -9 -6 -5 11.30 2.90 -2 8 -4 2.00 2.60 3 -6 4 12.50 2.50 -3 6 -4 12.50 2.10 -3 6 -4 14.40 2.70 4 -4 4 108.69 5.40 4 -4 4 115.69 6.00 -4 4 -4 103.49 5.20 -4 4 -4 108.69 5.80 -4 4 -4 113.49 5.90 5 -2 4 146.09 6.60 5 -2 4 128.59 6.00 -5 2 -4 127.89 6.10 -5 2 -4 127.79 5.90 -5 2 -4 125.69 5.30 6 0 4 6.00 1.50 6 0 4 3.20 1.40 -6 0 -4 3.60 1.30 -6 0 -4 3.80 1.30 -6 0 -4 2.90 1.00 -6 0 -4 2.60 0.80 7 2 4 259.77 10.10 7 2 4 250.77 10.20 -7 -2 -4 243.88 10.50 -7 -2 -4 272.87 10.50 8 4 4 2.40 1.60 8 4 4 2.20 1.40 -8 -4 -4 1.80 0.60 -8 -4 -4 2.60 1.50 -8 -4 -4 3.10 1.70 9 6 4 0.90 2.10 -9 -6 -4 -0.60 2.00 2 -8 3 17.70 3.20 -2 8 -3 15.10 3.30 3 -6 3 7.10 2.00 -3 6 -3 4.50 1.90 -3 6 -3 1.00 1.70 4 -4 3 34.50 3.50 4 -4 3 37.50 3.00 -4 4 -3 30.80 3.20 -4 4 -3 28.60 3.10 -4 4 -3 35.20 2.80 5 -2 3 6.40 1.70 5 -2 3 2.40 1.10 -5 2 -3 1.40 1.20 -5 2 -3 4.60 1.30 -5 2 -3 2.30 1.10 -5 2 -3 2.50 1.00 6 0 3 20.50 2.20 6 0 3 23.10 2.40 -6 0 -3 19.50 2.50 -6 0 -3 17.10 1.80 -6 0 -3 19.30 2.20 -6 0 -3 29.00 1.80 7 2 3 55.89 3.60 -7 -2 -3 55.09 2.90 -7 -2 -3 50.99 4.20 -7 -2 -3 52.69 3.60 8 4 3 115.69 6.20 -8 -4 -3 109.89 4.70 -8 -4 -3 130.89 6.10 -8 -4 -3 108.09 6.30 9 6 3 5.40 2.40 -9 -6 -3 5.10 1.30 -9 -6 -3 5.10 2.50 2 -8 2 2.30 2.20 -2 8 -2 2.50 2.40 3 -6 2 4.40 1.90 -3 6 -2 0.30 1.80 -3 6 -2 1.10 1.60 4 -4 2 158.68 7.40 4 -4 2 159.58 6.70 -4 4 -2 156.98 7.20 -4 4 -2 156.88 7.60 -4 4 -2 155.18 6.60 -4 4 -2 153.98 6.80 5 -2 2 76.29 4.40 5 -2 2 79.99 4.20 -5 2 -2 83.49 4.70 -5 2 -2 74.69 4.30 -5 2 -2 82.29 4.30 -5 2 -2 84.79 3.80 6 0 2 11.90 1.80 6 0 2 18.00 2.10 -6 0 -2 13.60 2.10 -6 0 -2 11.20 1.30 -6 0 -2 11.50 2.00 -6 0 -2 11.70 1.60 7 2 2 18.00 2.20 -7 -2 -2 16.60 2.50 -7 -2 -2 19.60 2.00 -7 -2 -2 13.60 2.10 8 4 2 6.40 2.00 -8 -4 -2 5.50 2.00 -8 -4 -2 5.10 1.70 -8 -4 -2 5.70 1.40 9 6 2 2.30 2.40 -9 -6 -2 -0.70 2.10 -9 -6 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54.59 4.50 4 -6 4 -0.60 1.80 -4 6 -4 1.20 2.30 -4 6 -4 0.10 2.00 5 -4 4 136.99 6.80 5 -4 4 134.79 7.40 -5 4 -4 136.39 7.40 -5 4 -4 144.69 6.50 -5 4 -4 148.99 7.30 -5 4 -4 144.59 6.90 6 -2 4 10.90 2.20 6 -2 4 12.70 2.10 -6 2 -4 8.00 2.00 -6 2 -4 11.00 1.90 -6 2 -4 7.60 1.90 -6 2 -4 7.90 1.60 7 0 4 -1.00 1.30 7 0 4 0.30 1.40 -7 0 -4 -0.30 1.00 -7 0 -4 0.10 0.90 -7 0 -4 1.20 1.30 -7 0 -4 0.30 1.30 8 2 4 36.50 3.50 -8 -2 -4 35.10 3.50 -8 -2 -4 34.70 3.80 -9 -4 -4 23.10 3.10 -9 -4 -4 15.30 1.50 -9 -4 -4 16.50 3.20 4 -6 3 -0.20 1.90 -4 6 -3 0.90 2.10 -4 6 -3 -0.50 2.00 5 -4 3 30.20 3.10 5 -4 3 41.20 4.00 -5 4 -3 35.80 3.00 -5 4 -3 41.80 3.90 -5 4 -3 32.10 3.30 -5 4 -3 25.60 3.40 6 -2 3 36.30 3.20 6 -2 3 34.40 3.50 -6 2 -3 29.30 3.40 -6 2 -3 22.50 2.40 -6 2 -3 23.70 2.70 -6 2 -3 27.00 3.10 7 0 3 0.70 1.30 7 0 3 2.50 1.40 -7 0 -3 2.80 1.60 -7 0 -3 0.90 1.40 -7 0 -3 1.30 1.10 -7 0 -3 1.60 1.20 8 2 3 135.09 6.90 -8 -2 -3 147.29 7.20 -8 -2 -3 147.89 6.20 -8 -2 -3 143.59 7.50 -9 -4 -3 4.70 2.10 -9 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2.20 -5 5 -2 2.60 1.90 6 -3 2 40.90 3.60 6 -3 2 41.50 4.00 -6 3 -2 44.80 3.90 -6 3 -2 23.50 3.10 -6 3 -2 26.80 2.90 -6 3 -2 31.20 3.70 7 -1 2 23.70 2.90 -7 1 -2 23.60 3.00 -7 1 -2 30.60 3.80 -7 1 -2 22.80 2.40 -7 1 -2 27.50 3.00 -8 -1 -2 12.50 2.40 -8 -1 -2 10.90 2.70 -8 -1 -2 14.70 2.30 -8 -1 -2 9.30 1.60 -9 -3 -2 10.10 2.90 -9 -3 -2 9.90 2.70 -9 -3 -2 9.40 2.00 5 -5 1 106.39 6.60 -5 5 -1 107.49 5.80 -5 5 -1 95.49 6.80 6 -3 1 24.60 3.20 -6 3 -1 13.30 2.60 -6 3 -1 12.80 2.90 -6 3 -1 20.00 2.40 -6 3 -1 22.90 3.10 -7 1 -1 0.00 1.60 -7 1 -1 -0.80 1.50 -7 1 -1 -0.10 1.30 -7 1 -1 1.60 1.90 -8 -1 -1 18.60 3.30 -8 -1 -1 16.10 2.50 -8 -1 -1 23.50 3.20 -8 -1 -1 18.50 2.10 -9 -3 -1 33.20 4.50 -9 -3 -1 26.80 2.60 -9 -3 -1 26.50 3.10 -9 -3 -1 23.50 3.50 5 -5 0 4.40 2.70 -5 5 0 11.80 3.40 -6 3 0 14.40 3.20 -6 3 0 10.40 2.60 -6 3 0 16.20 2.50 -6 3 0 11.40 2.50 -7 1 0 44.30 4.60 -7 1 0 58.19 4.40 -7 1 0 58.89 3.90 -7 1 0 51.49 4.50 -8 -1 0 49.50 4.50 -8 -1 0 46.80 3.40 -8 -1 0 38.30 4.60 -8 -1 0 41.80 4.10 5 -5 -1 7.30 2.90 -6 3 1 96.09 6.00 -6 3 1 94.49 6.60 -6 3 1 95.09 5.50 -7 1 1 6.10 2.10 -7 1 1 9.30 2.60 -7 1 1 8.60 2.80 -7 1 1 4.80 2.40 -8 -1 1 0.30 2.30 -8 -1 1 3.60 2.30 -8 -1 1 0.60 1.80 -8 -1 1 0.60 2.40 -6 3 2 19.50 3.00 -6 3 2 17.20 3.70 -7 1 2 -1.40 2.10 -7 1 2 3.20 2.20 -7 1 2 -0.50 2.40 -7 1 2 2.00 2.70 8 0 7 6.10 2.90 -8 0 -7 3.70 1.70 6 -4 6 54.39 7.10 7 -2 6 1.30 2.10 7 -2 6 -0.10 2.10 -7 2 -6 -1.60 1.70 -7 2 -6 -0.10 1.90 -7 2 -6 0.90 1.70 8 0 6 5.40 2.60 8 0 6 4.90 2.30 -8 0 -6 1.50 2.00 -8 0 -6 2.90 1.70 -8 0 -6 4.00 1.80 6 -4 5 14.10 3.10 6 -4 5 8.30 2.50 -6 4 -5 9.80 3.00 -6 4 -5 14.40 2.80 -6 4 -5 14.10 3.00 7 -2 5 0.90 1.90 7 -2 5 1.10 2.10 -7 2 -5 3.20 2.20 -7 2 -5 2.20 1.90 -7 2 -5 2.20 1.90 -7 2 -5 -0.80 1.80 8 0 5 0.40 2.10 8 0 5 5.20 2.20 -8 0 -5 2.20 1.50 -8 0 -5 1.60 1.90 -8 0 -5 2.00 2.10 -8 0 -5 1.50 1.50 9 2 5 70.49 5.40 -9 -2 -5 69.79 5.50 -9 -2 -5 59.79 3.60 -9 -2 -5 54.79 7.10 6 -4 4 2.20 1.90 6 -4 4 3.90 2.40 -6 4 -4 1.30 1.90 -6 4 -4 3.40 2.20 -6 4 -4 1.60 2.20 -6 4 -4 -0.40 2.10 7 -2 4 7.00 2.20 7 -2 4 4.20 2.30 -7 2 -4 1.90 1.70 -7 2 -4 1.90 1.80 -7 2 -4 3.20 2.10 -7 2 -4 4.10 2.10 8 0 4 13.10 2.60 -8 0 -4 20.30 2.20 -8 0 -4 11.50 2.80 -8 0 -4 11.40 2.10 -8 0 -4 19.40 3.10 9 2 4 7.30 2.50 -9 -2 -4 8.40 2.60 -9 -2 -4 3.70 1.40 -9 -2 -4 8.30 2.70 6 -4 3 26.90 3.30 6 -4 3 34.40 4.20 -6 4 -3 16.20 3.30 -6 4 -3 22.50 3.30 -6 4 -3 20.20 2.90 -6 4 -3 23.60 3.40 7 -2 3 18.90 2.90 7 -2 3 33.30 3.80 -7 2 -3 28.40 2.70 -7 2 -3 25.10 3.40 -7 2 -3 26.90 3.30 -7 2 -3 16.40 2.70 8 0 3 0.80 1.70 -8 0 -3 -0.40 1.40 -8 0 -3 2.60 1.90 -8 0 -3 -0.60 1.40 -8 0 -3 -0.60 1.70 -9 -2 -3 0.30 2.20 -9 -2 -3 3.80 1.60 -9 -2 -3 -0.60 2.50 -9 -2 -3 1.40 2.10 6 -4 2 25.20 3.10 6 -4 2 27.80 3.70 -6 4 -2 17.20 3.10 -6 4 -2 23.20 3.70 -6 4 -2 18.60 2.70 -6 4 -2 21.60 3.20 7 -2 2 48.50 4.30 -7 2 -2 43.60 4.30 -7 2 -2 32.00 4.10 -7 2 -2 51.49 3.80 -8 0 -2 3.40 1.80 -8 0 -2 1.10 1.90 -8 0 -2 -0.20 1.90 -8 0 -2 0.40 1.50 -9 -2 -2 0.00 1.50 -9 -2 -2 -2.20 2.00 -9 -2 -2 4.10 2.70 -9 -2 -2 1.80 1.90 6 -4 1 3.00 2.60 -6 4 -1 4.40 2.20 -6 4 -1 2.40 2.40 -6 4 -1 0.80 2.70 -7 2 -1 137.19 6.40 -7 2 -1 126.39 7.00 -7 2 -1 113.29 7.50 -7 2 -1 137.69 7.20 -8 0 -1 23.10 3.50 -8 0 -1 25.00 3.80 -8 0 -1 27.30 3.50 -8 0 -1 24.60 2.80 -9 -2 -1 8.40 2.50 -6 4 0 4.00 2.10 -7 2 0 203.78 9.50 -7 2 0 185.98 10.00 -7 2 0 202.98 8.60 -7 2 0 187.58 9.30 -8 0 0 7.00 2.70 -8 0 0 0.70 2.40 -8 0 0 4.20 1.90 -8 0 0 1.20 2.00 -7 2 1 16.90 3.10 -7 2 1 7.90 3.10 -7 2 1 2.50 2.60 8 -1 6 12.20 4.90 8 -1 5 40.10 4.50 -8 1 -5 37.80 3.60 7 -3 4 1.00 2.30 7 -3 4 3.20 2.30 -7 3 -4 2.30 2.60 -7 3 -4 2.10 2.40 -7 3 -4 2.60 2.40 8 -1 4 13.90 3.00 -8 1 -4 17.90 3.20 -8 1 -4 9.60 2.80 -8 1 -4 14.70 2.50 -8 1 -4 14.20 2.90 -9 -1 -4 10.50 2.00 -9 -1 -4 8.20 2.80 7 -3 3 10.10 2.70 7 -3 3 12.50 3.40 -7 3 -3 9.60 2.60 -7 3 -3 13.80 3.00 -7 3 -3 11.10 3.00 8 -1 3 20.30 3.30 -8 1 -3 17.20 2.80 -8 1 -3 21.30 2.80 -8 1 -3 13.40 3.10 -8 1 -3 16.30 3.10 -9 -1 -3 12.50 2.30 -7 3 -2 0.20 2.10 -7 3 -2 1.80 2.50 -8 1 -2 27.30 4.60 -8 1 -2 33.10 3.80 -8 1 -2 33.50 4.20 -7 3 -1 29.00 4.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6193 _shelx_res_file ; TITL berry976_a.res in P-1 berry976.res created by SHELXL-2018/1 at 09:51:36 on 19-Aug-2019 REM Old TITL Berry976a in P-1 REM SHELXT solution in P-1 REM R1 0.115, Rweak 0.005, Alpha 0.055, Orientation as input REM Formula found by SHELXT: C5 N3 CELL 0.71073 6.3296 7.0222 7.3512 84.975 71.693 63.889 ZERR 2 0.0019 0.0019 0.0021 0.013 0.013 0.012 LATT 1 SFAC C H N O UNIT 10 16 4 2 EQIV $1 -X,1-Y,1-Z EQIV $2 +X,-1+Y,+Z L.S. 24 PLAN 20 SIZE 0.161 0.051 0.01 TEMP -173.15 HTAB N2 N1_$1 HTAB N2 O1_$2 BOND $H CONF ACTA 50 list 4 fmap 2 53 OMIT 0 0 7 REM REM REM WGHT 0.054400 0.104300 FVAR 1.40051 O1 4 0.379740 0.778537 0.289002 11.00000 0.02418 0.01195 = 0.02172 -0.00074 -0.00363 -0.00924 N1 3 0.294684 0.496624 0.361155 11.00000 0.01268 0.01066 = 0.01405 -0.00073 -0.00245 -0.00562 N2 3 0.213261 0.208399 0.416223 11.00000 0.01243 0.01041 = 0.01983 -0.00161 -0.00257 -0.00554 H2A 2 0.061163 0.294549 0.485888 11.00000 -1.20000 H2B 2 0.256360 0.070526 0.390399 11.00000 -1.20000 C1 1 0.455047 0.583433 0.277513 11.00000 0.01567 0.01293 = 0.01125 -0.00046 -0.00309 -0.00733 C2 1 0.724392 0.446435 0.169052 11.00000 0.01506 0.01770 = 0.01477 -0.00165 -0.00018 -0.00971 AFIX 23 H2C 2 0.828777 0.499108 0.204319 11.00000 -1.20000 H2D 2 0.749196 0.461186 0.029656 11.00000 -1.20000 AFIX 0 C3 1 0.809095 0.212592 0.209603 11.00000 0.01065 0.01574 = 0.01710 -0.00366 -0.00195 -0.00515 AFIX 23 H3A 2 0.828669 0.190240 0.339314 11.00000 -1.20000 H3B 2 0.970881 0.126647 0.114773 11.00000 -1.20000 AFIX 0 C4 1 0.616858 0.143930 0.196914 11.00000 0.01243 0.01160 = 0.01453 -0.00317 -0.00203 -0.00434 AFIX 23 H4A 2 0.610844 0.150894 0.063433 11.00000 -1.20000 H4B 2 0.661582 -0.004411 0.234345 11.00000 -1.20000 AFIX 0 C5 1 0.368177 0.289654 0.329516 11.00000 0.01139 0.01140 = 0.01183 -0.00014 -0.00427 -0.00461 HKLF 4 REM berry976_a.res in P-1 REM R1 = 0.0426 for 1680 Fo > 4sig(Fo) and 0.0550 for all 2048 data REM 79 parameters refined using 0 restraints END WGHT 0.0544 0.1043 REM Highest difference peak 0.442, deepest hole -0.267, 1-sigma level 0.055 Q1 1 0.4975 0.2288 0.2637 11.00000 0.05 0.44 Q2 1 0.5987 0.5153 0.2242 11.00000 0.05 0.40 Q3 1 0.3693 0.5442 0.3189 11.00000 0.05 0.39 Q4 1 0.3696 0.3876 0.3478 11.00000 0.05 0.37 Q5 1 0.2809 0.2600 0.3720 11.00000 0.05 0.36 Q6 1 0.6988 0.1981 0.1876 11.00000 0.05 0.35 Q7 1 0.7973 0.3194 0.1759 11.00000 0.05 0.29 Q8 1 0.4442 0.6792 0.3035 11.00000 0.05 0.20 Q9 1 0.1853 0.5556 0.3421 11.00000 0.05 0.19 Q10 1 0.3585 0.6966 0.2870 11.00000 0.05 0.19 Q11 1 0.9456 0.1006 0.2046 11.00000 0.05 0.18 Q12 1 0.6144 0.0152 0.1933 11.00000 0.05 0.18 Q13 1 0.2365 0.8223 0.3543 11.00000 0.05 0.18 Q14 1 0.1994 0.5939 0.4591 11.00000 0.05 0.17 Q15 1 0.1495 0.5488 0.4395 11.00000 0.05 0.17 Q16 1 0.6404 0.3324 -0.0415 11.00000 0.05 0.16 Q17 1 0.5943 0.1790 0.1258 11.00000 0.05 0.16 Q18 1 0.7207 0.5228 -0.0176 11.00000 0.05 0.15 Q19 1 0.4638 0.8263 0.2757 11.00000 0.05 0.15 Q20 1 0.3422 0.2015 0.4478 11.00000 0.05 0.15 ; _shelx_res_checksum 5050 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.37974(15) 0.77854(12) 0.28900(12) 0.01953(18) Uani d 1 . . N N1 0.29468(15) 0.49662(13) 0.36116(12) 0.01259(17) Uani d 1 . . N N2 0.21326(16) 0.20840(14) 0.41622(13) 0.01446(18) Uani d 1 . . H H2A 0.061(3) 0.295(2) 0.486(2) 0.017 Uiso d 1 . . H H2B 0.256(3) 0.071(2) 0.390(2) 0.017 Uiso d 1 . . C C1 0.45505(18) 0.58343(16) 0.27751(14) 0.01306(19) Uani d 1 . . C C2 0.72439(18) 0.44644(17) 0.16905(15) 0.0158(2) Uani d 1 . . H H2C 0.828777 0.499108 0.204319 0.019 Uiso calc 1 . . H H2D 0.749196 0.461186 0.029656 0.019 Uiso calc 1 . . C C3 0.80909(17) 0.21259(16) 0.20960(15) 0.0150(2) Uani d 1 . . H H3A 0.828669 0.190240 0.339314 0.018 Uiso calc 1 . . H H3B 0.970881 0.126647 0.114773 0.018 Uiso calc 1 . . C C4 0.61686(17) 0.14393(15) 0.19691(14) 0.01348(19) Uani d 1 . . H H4A 0.610844 0.150894 0.063433 0.016 Uiso calc 1 . . H H4B 0.661582 -0.004411 0.234345 0.016 Uiso calc 1 . . C C5 0.36818(17) 0.28965(15) 0.32952(13) 0.01144(18) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0242(4) 0.0119(3) 0.0217(4) -0.0092(3) -0.0036(3) -0.0007(3) N1 0.0127(3) 0.0107(4) 0.0140(4) -0.0056(3) -0.0025(3) -0.0007(3) N2 0.0124(4) 0.0104(4) 0.0198(4) -0.0055(3) -0.0026(3) -0.0016(3) C1 0.0157(4) 0.0129(4) 0.0113(4) -0.0073(3) -0.0031(3) -0.0005(3) C2 0.0151(4) 0.0177(5) 0.0148(4) -0.0097(4) -0.0002(3) -0.0017(3) C3 0.0106(4) 0.0157(4) 0.0171(4) -0.0052(3) -0.0020(3) -0.0037(3) C4 0.0124(4) 0.0116(4) 0.0145(4) -0.0043(3) -0.0020(3) -0.0032(3) C5 0.0114(4) 0.0114(4) 0.0118(4) -0.0046(3) -0.0043(3) -0.0001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 N1 C1 . . 119.36(9) ? H2A N2 H2B . . 121.2(14) ? C5 N2 H2A . . 118.9(9) ? C5 N2 H2B . . 119.3(9) ? O1 C1 N1 . . 119.52(9) ? O1 C1 C2 . . 118.85(9) ? N1 C1 C2 . . 121.63(9) ? C1 C2 H2C . . 108.9 ? C1 C2 H2D . . 108.9 ? C1 C2 C3 . . 113.27(8) ? H2C C2 H2D . . 107.7 ? C3 C2 H2C . . 108.9 ? C3 C2 H2D . . 108.9 ? C2 C3 H3A . . 109.9 ? C2 C3 H3B . . 109.9 ? C2 C3 C4 . . 108.86(8) ? H3A C3 H3B . . 108.3 ? C4 C3 H3A . . 109.9 ? C4 C3 H3B . . 109.9 ? C3 C4 H4A . . 109.9 ? C3 C4 H4B . . 109.9 ? H4A C4 H4B . . 108.3 ? C5 C4 C3 . . 108.86(8) ? C5 C4 H4A . . 109.9 ? C5 C4 H4B . . 109.9 ? N1 C5 C4 . . 123.80(8) ? N2 C5 N1 . . 118.26(9) ? N2 C5 C4 . . 117.93(9) ? 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 C1 . 1.2376(12) ? N1 C1 . 1.3663(13) ? N1 C5 . 1.3338(13) ? N2 H2A . 0.887(16) ? N2 H2B . 0.903(15) ? N2 C5 . 1.3151(13) ? C1 C2 . 1.5180(15) ? C2 H2C . 0.9900 ? C2 H2D . 0.9900 ? C2 C3 . 1.5207(15) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C3 C4 . 1.5223(14) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C4 C5 . 1.5060(14) ? 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 N2 H2A N1 2_566 0.887(16) 2.068(16) 2.9550(15) 177.6(13) yes N2 H2B O1 1_545 0.903(15) 1.965(16) 2.8588(14) 170.1(14) 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 O1 C1 C2 C3 . . . . 164.67(9) ? N1 C1 C2 C3 . . . . -15.73(13) ? C1 N1 C5 N2 . . . . 177.95(8) ? C1 N1 C5 C4 . . . . -3.33(14) ? C1 C2 C3 C4 . . . . 46.55(11) ? C2 C3 C4 C5 . . . . -54.51(11) ? C3 C4 C5 N1 . . . . 35.61(12) ? C3 C4 C5 N2 . . . . -145.67(9) ? C5 N1 C1 O1 . . . . 172.09(9) ? C5 N1 C1 C2 . . . . -7.50(14) ? _cod_database_fobs_code 2022703