#------------------------------------------------------------------------------ #$Date: 2023-07-06 20:17:42 +0200 (Thu, 06 Jul 2023) $ #$Revision: 285049 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022760.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_2022760 loop_ _publ_author_name 'Hong, Dabeen' 'Lee, Kyounghoon' _publ_section_title ; Polymorphic structures of 3-phenyl-1H-1,3-benzo-diazol-2(3H)-one. ; _journal_coeditor_code VM2281 _journal_issue 'Pt 6' _journal_name_full 'Acta crystallographica. Section E, Crystallographic communications' _journal_page_first 534 _journal_page_last 537 _journal_paper_doi 10.1107/S2056989023003961 _journal_volume 79 _journal_year 2023 _chemical_formula_moiety 'C13 H10 N2 O' _chemical_formula_sum 'C13 H10 N2 O' _chemical_formula_weight 210.23 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 13.7925(3) _cell_length_b 7.26520(10) _cell_length_c 19.7956(4) _cell_measurement_reflns_used 9912 _cell_measurement_temperature 193.15 _cell_measurement_theta_max 28.262 _cell_measurement_theta_min 2.533 _cell_volume 1983.62(6) _computing_cell_refinement ; SAINT (Bruker, 2012) ; _computing_data_collection ; APEX2 (Bruker, 2012) ; _computing_data_reduction ; SAINT (Bruker, 2012) ; _computing_molecular_graphics ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 193.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_unetI/netI 0.0153 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 34068 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.360 _diffrn_reflns_theta_min 2.058 _diffrn_source_current 18.0 _diffrn_source_power 0.9 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.7122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.408 _exptl_crystal_description BLOCK _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.329 _exptl_crystal_size_min 0.188 _refine_diff_density_max 0.245 _refine_diff_density_min -0.375 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2479 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0391 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+1.3866P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0955 _refine_ls_wR_factor_ref 0.0989 _reflns_number_gt 2203 _reflns_number_total 2479 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vm2281sup1.cif _cod_data_source_block II _cod_depositor_comments 'Adding full bibliography for 2022759--2022760.cif.' _cod_database_code 2022760 _cod_database_fobs_code 2022760 _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 0.967 _shelx_estimated_absorpt_t_max 0.983 _shelx_hkl_file ; 0 -1 0 -0.10 0.20 0 1 0 -0.10 0.20 0 1 0 -0.10 0.10 0 -2 0 58.59 2.60 0 2 0 64.99 2.70 0 2 0 64.79 1.70 0 2 0 60.39 2.60 0 2 0 59.39 1.70 0 -3 0 -1.10 0.30 0 3 0 -0.80 0.20 0 3 0 -0.70 0.50 0 3 0 -0.30 0.50 0 3 0 -1.10 0.20 0 -4 0 101.49 4.80 0 4 0 106.69 4.80 0 4 0 109.29 3.10 0 4 0 105.19 3.10 0 4 0 104.39 4.80 0 -5 0 0.80 0.80 0 5 0 -0.60 0.50 0 5 0 -0.40 0.50 0 5 0 0.40 0.30 0 5 0 -0.10 0.20 0 5 0 0.20 0.20 0 -6 0 625.84 19.40 0 6 0 632.24 15.50 0 6 0 644.64 15.30 0 6 0 643.54 15.50 0 6 0 648.94 18.90 0 6 0 654.93 19.30 0 -7 0 0.60 1.30 0 7 0 1.10 1.30 0 7 0 0.40 0.40 0 7 0 -0.40 0.40 0 7 0 -0.40 0.90 0 7 0 0.70 0.40 0 -8 0 65.99 6.40 0 8 0 62.29 2.80 0 9 0 0.40 0.60 -1 9 0 -0.60 0.50 -1 8 0 0.50 0.40 -1 8 0 0.00 0.50 -1 8 0 0.40 0.40 1 -8 0 0.50 1.20 -1 7 0 -0.30 0.40 -1 7 0 0.10 0.40 -1 7 0 -0.10 1.10 -1 7 0 0.30 0.50 -1 7 0 1.40 1.10 1 -7 0 0.40 1.10 -1 6 0 -0.10 0.30 -1 6 0 1.60 1.00 -1 6 0 1.50 0.60 -1 6 0 0.10 0.90 -1 6 0 0.10 0.30 1 -6 0 0.00 0.80 -1 5 0 0.20 0.30 -1 5 0 -0.50 0.60 -1 5 0 -0.10 0.30 -1 5 0 0.40 0.30 -1 5 0 0.10 0.70 -1 5 0 0.30 0.30 1 -5 0 -1.30 0.50 -1 4 0 -0.50 0.40 -1 4 0 -0.20 0.20 -1 4 0 0.20 0.60 -1 4 0 0.00 0.20 -1 4 0 -0.10 0.30 -1 4 0 0.50 0.30 1 -4 0 0.00 0.50 -1 3 0 -0.20 0.20 -1 3 0 -0.20 0.20 -1 3 0 -0.50 0.40 -1 3 0 -0.30 0.20 -1 3 0 -0.50 0.40 -1 3 0 -0.50 0.20 -1 2 0 0.30 0.30 -1 2 0 1.00 0.30 -1 2 0 0.20 0.20 -1 2 0 0.20 0.10 -1 2 0 -0.10 0.30 -1 2 0 -0.20 0.10 -1 1 0 -1.30 0.10 -1 1 0 -1.00 0.20 -1 1 0 -1.30 0.10 -1 1 0 -1.40 0.10 1 -1 0 -1.40 0.10 1 -1 0 -1.10 0.10 -1 0 0 -0.80 0.10 -1 0 0 -0.70 0.10 -1 0 0 -0.60 0.10 -1 0 0 -0.80 0.10 1 0 0 -0.70 0.10 1 0 0 -0.80 0.10 1 0 0 -0.80 0.10 1 0 0 -0.70 0.10 -1 -1 0 -1.50 0.20 1 1 0 -1.30 0.10 1 1 0 -1.30 0.10 1 1 0 -1.30 0.10 1 1 0 -1.30 0.20 1 1 0 -1.30 0.20 -1 -2 0 0.20 0.40 1 2 0 -0.70 0.30 1 2 0 0.00 0.10 1 2 0 0.30 0.20 1 2 0 -0.10 0.30 1 2 0 0.00 0.10 -1 -3 0 -0.70 0.30 1 3 0 0.10 0.60 1 3 0 -0.60 0.40 1 3 0 -0.30 0.20 1 3 0 -0.20 0.20 -1 -4 0 0.10 0.50 1 4 0 0.00 0.50 1 4 0 -0.30 0.60 1 4 0 0.00 0.20 1 4 0 0.10 0.20 1 4 0 0.00 0.20 -1 -5 0 0.00 0.60 1 5 0 0.10 0.30 1 5 0 0.40 0.80 1 5 0 0.80 0.90 1 5 0 0.20 0.30 1 5 0 0.10 0.20 -1 -6 0 1.40 1.10 1 6 0 0.90 1.00 1 6 0 0.40 1.00 1 6 0 -0.30 0.30 1 6 0 -0.70 0.30 1 6 0 -0.30 0.30 -1 -7 0 1.10 1.20 1 7 0 0.10 0.50 1 7 0 0.00 0.40 1 7 0 -1.80 0.90 1 7 0 0.80 1.20 1 7 0 0.10 0.40 -1 -8 0 -1.00 1.20 1 8 0 1.20 1.40 1 8 0 -0.40 0.50 1 9 0 -0.10 0.50 -2 9 0 -0.10 0.60 -2 8 0 15.90 1.60 -2 8 0 18.50 1.90 2 -8 0 18.00 3.50 -2 7 0 628.04 16.30 -2 7 0 634.84 16.20 -2 7 0 655.63 16.10 2 -7 0 638.04 20.40 -2 6 0 263.77 7.50 -2 6 0 256.37 9.60 -2 6 0 265.67 7.70 -2 6 0 254.77 7.90 -2 6 0 258.07 7.70 -2 6 0 270.97 9.20 2 -6 0 268.17 10.50 -2 5 0 41.60 2.30 -2 5 0 42.20 2.00 -2 5 0 39.70 2.20 -2 5 0 45.40 3.10 -2 5 0 45.10 2.90 -2 5 0 42.20 2.20 2 -5 0 46.30 3.50 -2 4 0 10.50 1.20 -2 4 0 6.90 1.00 -2 4 0 7.20 1.20 -2 4 0 7.60 1.10 -2 4 0 9.40 1.50 -2 4 0 8.00 0.90 -2 3 0 2445.16 56.39 -2 3 0 2426.96 56.19 -2 3 0 2486.85 56.29 -2 3 0 2531.55 56.59 -2 3 0 2510.15 56.19 -2 3 0 2461.25 56.99 -2 2 0 853.81 20.40 -2 2 0 865.41 20.50 -2 2 0 851.11 20.30 -2 2 0 864.11 20.60 -2 2 0 874.11 20.10 -2 2 0 842.82 19.80 -2 1 0 4780.32 117.99 -2 1 0 4766.22 122.29 -2 1 0 4947.31 110.09 -2 1 0 4616.14 109.69 2 -1 0 4901.81 113.39 2 -1 0 4809.32 112.79 2 -1 0 4904.61 115.79 2 -1 0 4748.12 114.29 -2 0 0 493.45 11.60 -2 0 0 491.35 11.80 -2 0 0 485.05 12.30 -2 0 0 482.25 12.00 2 0 0 493.85 11.60 2 0 0 486.35 11.70 2 0 0 476.55 12.00 2 0 0 472.55 12.20 -2 -1 0 4702.43 115.89 -2 -1 0 4946.51 118.89 2 1 0 4862.41 120.89 2 1 0 5554.34 113.19 -2 -2 0 864.11 21.20 2 2 0 884.41 20.70 2 2 0 874.71 20.40 2 2 0 844.22 20.40 2 2 0 870.21 21.10 2 2 0 867.01 21.70 2 2 0 870.41 20.00 -2 -3 0 2417.26 56.59 2 3 0 2439.46 55.29 2 3 0 2456.85 54.69 2 3 0 2460.25 57.29 2 3 0 2495.85 54.99 2 3 0 2444.66 56.69 2 3 0 2391.46 57.09 2 3 0 2354.26 54.99 -2 -4 0 10.90 1.80 2 4 0 10.50 1.20 2 4 0 8.70 1.00 2 4 0 9.20 1.00 2 4 0 10.70 2.00 2 4 0 8.90 1.80 -2 -5 0 45.50 3.50 2 5 0 42.70 2.10 2 5 0 48.90 3.80 2 5 0 47.20 4.40 2 5 0 47.20 2.10 2 5 0 45.30 2.10 -2 -6 0 265.27 10.40 2 6 0 262.07 7.60 2 6 0 269.97 10.70 2 6 0 268.27 7.40 2 6 0 254.27 10.40 2 6 0 262.07 7.30 -2 -7 0 653.43 20.30 2 7 0 632.34 16.30 2 7 0 623.74 15.40 2 7 0 640.14 20.40 2 7 0 640.74 15.70 2 7 0 631.34 15.60 -2 -8 0 21.30 3.90 2 8 0 17.10 3.30 2 8 0 20.40 2.00 2 9 0 0.70 0.70 -3 9 0 0.70 0.80 -3 9 0 0.10 0.60 -3 8 0 0.00 0.70 -3 8 0 -0.10 0.60 3 -8 0 0.20 1.50 -3 7 0 0.60 0.60 -3 7 0 -0.70 0.50 3 -7 0 0.40 1.20 -3 6 0 0.30 0.60 -3 6 0 0.40 0.60 -3 6 0 0.30 0.80 -3 6 0 -0.30 0.40 -3 6 0 0.00 0.50 3 -6 0 0.10 1.10 -3 5 0 -0.40 0.40 -3 5 0 0.30 0.60 -3 5 0 -0.50 0.40 -3 5 0 0.20 0.50 -3 5 0 0.50 0.60 -3 5 0 -0.40 0.50 -3 4 0 -0.80 0.20 -3 4 0 -0.40 0.30 -3 4 0 -0.50 0.30 -3 4 0 0.00 0.40 -3 4 0 -0.10 0.40 -3 4 0 -0.20 0.30 -3 3 0 -0.10 0.40 -3 3 0 -0.40 0.30 -3 3 0 -0.70 0.30 -3 3 0 0.20 0.40 -3 3 0 -0.20 0.30 -3 2 0 -0.20 0.30 -3 2 0 0.00 0.30 -3 2 0 -0.10 0.30 3 -2 0 0.10 0.30 3 -2 0 0.20 0.20 3 -2 0 -0.10 0.10 3 -2 0 0.40 0.20 -3 1 0 0.00 0.40 -3 1 0 0.00 0.20 -3 1 0 -0.10 0.20 -3 1 0 -0.10 0.20 -3 1 0 0.00 0.10 -3 1 0 -0.10 0.40 -3 1 0 -0.40 0.30 3 -1 0 -0.10 0.30 3 -1 0 0.10 0.30 3 -1 0 0.90 0.40 3 -1 0 -0.10 0.40 -3 0 0 -0.30 0.30 -3 0 0 -0.70 0.30 -3 0 0 -0.40 0.30 -3 0 0 -0.30 0.30 3 0 0 -0.70 0.30 3 0 0 -0.50 0.30 3 0 0 -0.30 0.40 3 0 0 -0.40 0.40 3 0 0 -0.60 0.30 -3 -1 0 0.10 0.30 -3 -1 0 0.00 0.30 -3 -1 0 -0.40 0.20 3 1 0 0.60 0.20 3 1 0 -0.30 0.20 3 1 0 0.20 0.20 3 1 0 0.20 0.30 3 1 0 0.10 0.40 3 1 0 -0.10 0.40 3 2 0 0.10 0.30 3 2 0 0.60 0.40 3 2 0 -0.10 0.30 3 2 0 -0.10 0.30 3 2 0 0.10 0.20 -3 -3 0 -0.30 0.50 3 3 0 -0.10 0.40 3 3 0 -0.30 0.30 3 3 0 -0.20 0.30 3 3 0 -0.10 0.60 3 3 0 -0.20 0.30 -3 -4 0 -0.20 0.60 3 4 0 0.10 0.50 3 4 0 -0.40 0.20 3 4 0 -0.40 0.20 3 4 0 0.10 0.60 3 4 0 -0.10 0.40 -3 -5 0 0.40 0.80 3 5 0 1.30 0.50 3 5 0 0.30 0.30 3 5 0 0.10 0.40 3 5 0 -0.70 0.60 3 5 0 0.30 0.50 -3 -6 0 1.00 1.00 3 6 0 -0.20 1.00 3 6 0 0.40 0.50 3 6 0 0.30 0.40 3 6 0 -0.20 0.40 3 6 0 0.20 0.60 -3 -7 0 -0.40 1.10 3 7 0 0.20 0.60 3 7 0 0.40 1.30 3 7 0 0.30 0.50 3 7 0 0.90 0.60 -3 -8 0 0.40 1.40 3 8 0 -0.20 0.60 3 8 0 -1.90 1.10 3 8 0 -0.20 0.40 3 8 0 0.40 0.50 3 9 0 0.60 0.80 -4 9 0 57.39 3.70 -4 9 0 58.59 3.30 -4 8 0 29.10 2.80 -4 8 0 28.70 2.90 4 -8 0 35.60 5.80 -4 7 0 132.59 5.50 -4 7 0 123.59 5.30 4 -7 0 142.69 7.90 -4 6 0 117.89 5.70 -4 6 0 105.69 4.60 -4 6 0 108.29 4.80 -4 5 0 541.45 15.40 -4 5 0 530.65 14.70 -4 5 0 548.65 15.10 -4 5 0 526.35 15.10 -4 5 0 537.05 14.50 -4 4 0 584.34 16.00 -4 4 0 621.14 16.50 -4 4 0 627.24 15.90 -4 4 0 591.84 16.20 -4 4 0 602.14 16.50 -4 3 0 274.07 8.30 -4 3 0 257.57 8.60 -4 3 0 264.27 8.00 -4 3 0 274.37 8.70 4 -3 0 274.87 6.80 -4 2 0 165.78 5.80 -4 2 0 168.18 5.60 4 -2 0 171.38 4.20 4 -2 0 169.28 4.90 4 -2 0 173.38 5.00 4 -2 0 169.88 5.80 -4 1 0 8765.92 211.18 -4 1 0 8498.05 218.78 -4 1 0 8351.56 215.58 -4 1 0 8776.22 208.78 -4 1 0 8574.84 208.08 -4 1 0 8820.42 204.48 4 -1 0 8906.71 204.98 4 -1 0 8264.57 208.08 4 -1 0 8473.45 221.68 -4 0 0 6402.86 176.78 -4 0 0 6880.61 171.28 -4 0 0 7486.35 157.48 -4 0 0 6679.93 169.98 4 0 0 6724.63 173.38 4 0 0 6805.22 168.88 4 0 0 7400.46 158.68 4 0 0 7322.77 158.68 -4 -1 0 8522.95 212.48 -4 -1 0 8479.45 222.08 -4 -1 0 8747.12 217.68 4 1 0 9999.00 200.68 4 1 0 8862.51 209.28 4 1 0 8519.65 225.38 4 1 0 8842.71 213.88 -4 -2 0 171.68 4.60 -4 -2 0 172.68 5.10 4 2 0 164.18 5.50 4 2 0 173.08 6.20 4 2 0 172.88 5.90 4 2 0 165.48 5.90 4 3 0 274.87 8.40 4 3 0 273.17 8.60 4 3 0 266.97 7.80 4 3 0 270.67 8.20 4 4 0 597.74 15.40 4 4 0 594.54 16.10 4 4 0 615.14 18.30 4 4 0 613.04 15.90 4 4 0 623.54 16.40 -4 -5 0 515.15 16.20 4 5 0 535.05 14.30 4 5 0 510.45 17.00 4 5 0 554.74 14.10 4 5 0 536.25 14.70 4 5 0 545.15 14.70 -4 -6 0 109.69 6.30 4 6 0 107.29 4.50 4 6 0 114.59 4.90 4 6 0 109.69 4.40 4 6 0 111.59 6.90 4 6 0 118.29 4.80 -4 -7 0 113.29 7.00 4 7 0 133.39 7.90 4 7 0 136.09 5.10 4 7 0 138.99 5.70 -4 -8 0 40.00 5.00 4 8 0 34.60 5.00 4 8 0 30.70 3.00 4 8 0 28.40 2.00 4 9 0 60.09 3.70 -5 9 0 -0.60 0.80 -5 9 0 -0.30 0.90 -5 8 0 0.00 0.80 -5 8 0 -0.60 0.70 -5 7 0 0.90 0.80 -5 7 0 -0.60 0.70 -5 6 0 -0.50 0.60 -5 6 0 0.10 0.70 -5 6 0 -0.90 0.60 -5 5 0 -0.40 0.60 -5 5 0 0.10 0.60 -5 5 0 1.40 0.80 -5 5 0 2.70 1.10 -5 4 0 0.20 0.60 -5 4 0 1.30 0.80 -5 4 0 0.30 0.50 -5 4 0 1.00 0.70 -5 4 0 -0.50 0.60 5 -4 0 -0.10 0.30 -5 3 0 0.30 0.60 -5 3 0 0.20 0.50 -5 3 0 -0.10 0.50 5 -3 0 -0.30 0.30 5 -3 0 -0.10 0.40 -5 2 0 -0.10 0.40 -5 2 0 0.40 0.60 -5 2 0 0.20 0.20 -5 2 0 -0.10 0.20 -5 2 0 1.40 0.30 -5 2 0 -0.30 0.40 -5 2 0 0.00 0.10 5 -2 0 0.30 0.40 5 -2 0 -0.10 0.40 5 -2 0 -0.50 0.40 -5 1 0 -0.30 0.20 -5 1 0 0.30 0.50 -5 1 0 0.10 0.50 -5 1 0 -0.30 0.30 -5 1 0 -0.20 0.30 5 -1 0 -0.30 0.30 5 -1 0 -0.30 0.60 5 -1 0 0.20 0.60 -5 0 0 0.00 0.50 -5 0 0 0.70 0.60 -5 0 0 -0.20 0.40 -5 0 0 1.50 0.60 -5 0 0 1.00 0.70 5 0 0 0.40 0.40 5 0 0 0.60 0.70 5 0 0 0.00 0.40 5 0 0 -0.30 0.50 -5 -1 0 0.00 0.40 -5 -1 0 0.40 0.40 -5 -1 0 -0.70 0.30 5 1 0 0.00 0.40 5 1 0 -0.20 0.50 5 1 0 0.00 0.30 5 1 0 0.00 0.20 5 1 0 0.40 0.60 -5 -2 0 0.20 0.40 -5 -2 0 0.10 0.30 -5 -2 0 0.30 0.40 5 2 0 -0.20 0.20 5 2 0 0.50 0.70 5 2 0 1.00 0.80 -5 -3 0 0.10 0.30 5 3 0 0.30 0.60 5 3 0 0.30 0.60 5 3 0 0.90 0.60 5 3 0 0.40 0.50 -5 -4 0 -0.30 0.20 5 4 0 0.40 0.60 5 4 0 0.10 0.40 5 4 0 -0.10 0.50 5 4 0 -0.20 0.50 5 4 0 -0.30 0.70 5 5 0 1.00 0.80 5 5 0 1.10 0.70 5 5 0 0.80 0.60 5 5 0 -0.20 0.60 5 5 0 -0.30 0.90 5 6 0 0.00 1.20 5 6 0 -0.30 0.70 5 6 0 -1.00 0.50 5 7 0 -0.70 0.60 5 7 0 -0.70 1.10 5 7 0 0.10 0.70 5 8 0 -0.60 0.80 5 8 0 -0.60 1.30 5 8 0 0.30 0.70 5 9 0 0.50 0.90 5 9 0 0.70 0.60 -6 9 0 33.90 3.50 -6 9 0 32.80 3.60 -6 8 0 48.30 3.80 -6 8 0 54.99 4.00 -6 7 0 98.89 5.30 -6 7 0 100.89 5.50 -6 6 0 180.58 8.60 -6 6 0 193.08 7.80 -6 6 0 197.98 7.70 -6 5 0 31.00 3.20 -6 5 0 28.70 3.10 -6 5 0 35.00 3.40 -6 4 0 2.50 1.00 -6 4 0 1.40 0.80 -6 4 0 0.20 0.60 -6 4 0 -0.40 0.60 6 -4 0 1.20 0.60 -6 2 0 11.30 1.10 -6 2 0 13.90 1.90 -6 2 0 11.20 0.90 -6 2 0 11.80 0.80 -6 2 0 13.40 1.00 -6 2 0 14.10 2.30 -6 2 0 13.10 2.00 6 -2 0 16.80 1.70 6 -2 0 14.80 2.10 -6 1 0 62.49 3.10 -6 1 0 70.79 3.90 -6 1 0 68.49 3.70 -6 1 0 70.49 2.80 -6 1 0 73.59 3.10 6 -1 0 70.39 3.20 6 -1 0 78.69 4.40 6 -1 0 65.59 3.90 -6 0 0 331.97 10.20 -6 0 0 324.97 8.90 -6 0 0 314.07 9.80 -6 0 0 319.47 9.30 6 0 0 324.07 8.80 6 0 0 289.07 10.20 6 0 0 323.87 9.00 6 0 0 313.97 10.70 -6 -1 0 71.09 3.40 -6 -1 0 70.79 3.50 -6 -1 0 70.39 3.00 -6 -1 0 68.49 3.70 6 1 0 65.79 2.70 6 1 0 69.09 4.20 6 1 0 61.89 3.80 6 1 0 67.89 2.70 -6 -2 0 8.20 1.30 -6 -2 0 11.50 1.50 -6 -2 0 14.10 1.40 6 2 0 11.80 2.10 6 2 0 9.20 1.70 6 2 0 12.40 1.80 6 2 0 12.20 0.70 6 2 0 12.40 0.70 -6 -3 0 50.19 2.50 -6 -3 0 40.20 2.10 6 3 0 58.69 3.70 6 3 0 56.79 3.70 -6 -4 0 1.40 0.60 6 4 0 0.30 0.50 6 4 0 1.00 0.90 6 4 0 2.10 1.00 6 4 0 -0.10 0.60 6 4 0 -0.60 0.70 6 5 0 33.50 3.40 6 5 0 26.10 3.00 6 5 0 24.00 3.60 6 6 0 193.28 7.70 6 6 0 199.68 9.90 6 6 0 182.18 7.80 6 7 0 97.79 5.10 6 7 0 106.79 7.50 6 7 0 103.39 5.60 6 8 0 45.50 6.10 6 8 0 46.70 4.40 6 8 0 46.40 3.30 6 9 0 36.20 2.60 6 9 0 29.60 3.50 -7 8 0 0.90 1.10 -7 8 0 -0.40 1.00 -7 7 0 2.80 1.30 -7 7 0 1.30 1.10 -7 6 0 -0.30 0.80 -7 6 0 -0.10 0.80 -7 5 0 -0.50 0.60 -7 5 0 -0.30 0.70 -7 5 0 -1.60 0.50 -7 4 0 0.10 0.70 -7 4 0 0.20 0.70 -7 3 0 -0.90 0.50 -7 3 0 0.00 0.60 -7 3 0 0.60 0.80 7 -3 0 -0.60 0.60 7 -3 0 0.10 0.60 -7 2 0 -1.10 0.40 -7 2 0 -0.10 0.20 -7 2 0 -0.90 0.60 -7 2 0 -0.60 0.40 -7 2 0 0.00 0.20 -7 2 0 2.90 0.60 7 -2 0 -0.40 0.60 7 -2 0 0.40 0.60 -7 1 0 0.20 0.40 -7 1 0 -0.30 0.40 -7 1 0 0.10 0.50 -7 1 0 -0.20 0.60 -7 1 0 -0.50 0.40 7 -1 0 -0.40 0.40 7 -1 0 0.80 0.90 7 -1 0 -0.10 0.70 -7 0 0 3.60 1.00 -7 0 0 2.70 0.90 -7 0 0 2.80 1.00 -7 0 0 3.50 0.90 -7 0 0 2.30 0.70 7 0 0 3.10 1.10 7 0 0 1.40 0.60 7 0 0 1.70 0.70 7 0 0 4.20 1.30 -7 -1 0 0.30 0.70 -7 -1 0 -0.30 0.40 -7 -1 0 -0.20 0.50 -7 -1 0 -0.30 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1071.59 25.90 -8 1 0 1068.19 28.00 -8 1 0 1088.79 26.40 8 -1 0 1061.59 28.80 8 -1 0 1086.99 26.80 8 -1 0 1054.49 29.10 -8 0 0 102.59 5.40 -8 0 0 105.29 4.30 -8 0 0 111.49 4.90 -8 0 0 100.09 5.10 -8 0 0 109.49 4.90 8 0 0 103.19 4.40 8 0 0 104.09 5.80 8 0 0 106.79 6.10 -8 -1 0 1072.99 27.30 -8 -1 0 1073.69 28.20 -8 -1 0 1066.89 27.60 -8 -1 0 1083.09 26.40 8 1 0 1060.39 25.90 8 1 0 1080.69 25.90 8 1 0 1094.59 29.20 8 1 0 1044.20 29.30 -8 -2 0 621.34 17.00 -8 -2 0 612.44 16.20 -8 -2 0 587.84 16.90 8 2 0 610.34 15.00 8 2 0 638.94 18.90 8 2 0 621.04 15.10 8 2 0 617.44 19.00 8 2 0 619.14 15.30 -8 -3 0 18.70 2.30 -8 -3 0 16.20 1.80 8 3 0 13.90 2.50 8 3 0 15.80 2.70 8 3 0 16.70 2.80 8 4 0 56.69 4.40 8 4 0 44.70 4.90 8 4 0 40.70 4.30 8 5 0 119.29 7.50 8 5 0 120.59 6.70 8 5 0 123.39 6.70 8 6 0 0.60 1.30 8 6 0 0.30 1.00 8 6 0 -0.40 0.90 8 7 0 1.10 1.20 8 7 0 0.50 1.60 8 7 0 0.50 1.00 8 8 0 19.40 3.40 8 8 0 20.80 3.10 -9 8 0 0.30 1.20 -9 8 0 -1.20 1.00 -9 7 0 0.30 1.10 -9 7 0 -0.10 1.00 -9 6 0 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0 -0.30 1.00 9 6 0 -0.40 1.00 9 6 0 -0.30 0.90 9 6 0 -1.00 1.30 9 7 0 -0.20 1.10 9 7 0 -0.20 1.00 9 8 0 -1.10 1.00 9 8 0 0.00 1.30 -10 8 0 19.70 3.70 -10 8 0 17.90 3.40 -10 7 0 14.10 3.10 -10 7 0 10.80 2.60 -10 6 0 44.90 5.20 -10 6 0 39.20 4.60 -10 5 0 151.98 7.80 -10 5 0 144.69 8.00 -10 4 0 0.60 1.10 -10 4 0 0.80 1.10 -10 3 0 272.67 6.70 -10 3 0 275.87 11.20 -10 3 0 276.17 10.80 -10 3 0 266.07 7.10 10 -3 0 264.17 9.60 -10 2 0 23.30 3.50 -10 2 0 27.90 3.60 -10 2 0 27.40 1.90 -10 2 0 28.60 2.60 10 -2 0 27.80 1.90 10 -2 0 33.70 3.30 -10 1 0 137.49 5.90 -10 1 0 141.59 5.40 -10 1 0 136.09 6.80 -10 1 0 142.29 7.30 10 -1 0 124.79 7.20 10 -1 0 142.49 7.80 10 -1 0 138.49 6.00 -10 0 0 346.77 11.60 -10 0 0 359.66 13.00 -10 0 0 358.26 10.90 -10 0 0 364.26 12.50 10 0 0 362.16 13.90 10 0 0 390.36 13.90 10 0 0 346.37 10.90 -10 -1 0 137.69 6.30 -10 -1 0 142.29 7.30 -10 -1 0 152.08 6.60 -10 -1 0 136.99 5.70 -10 -1 0 144.49 6.70 10 1 0 139.79 7.70 10 1 0 136.29 5.30 10 1 0 136.49 7.80 -10 -2 0 30.00 3.30 -10 -2 0 27.00 2.80 10 2 0 29.60 1.90 10 2 0 23.50 3.60 10 2 0 37.30 4.80 -10 -3 0 260.77 8.90 -10 -3 0 277.77 11.70 10 3 0 268.17 11.70 10 3 0 255.77 11.20 10 3 0 289.77 11.90 10 4 0 0.50 1.20 10 4 0 0.40 1.40 10 4 0 0.90 1.20 10 5 0 155.28 9.10 10 5 0 152.88 8.50 10 5 0 146.59 8.30 10 6 0 43.20 5.10 10 6 0 40.20 5.70 10 6 0 53.39 5.90 10 7 0 11.10 2.80 10 7 0 13.60 3.10 10 8 0 17.20 3.60 10 8 0 23.60 3.70 -11 7 0 -0.10 1.30 -11 7 0 0.10 1.30 -11 6 0 1.00 1.30 -11 6 0 0.50 1.30 -11 5 0 2.90 1.60 -11 5 0 0.10 1.10 -11 4 0 0.50 1.10 -11 4 0 0.00 1.00 -11 3 0 -1.10 0.90 -11 3 0 0.00 0.40 -11 3 0 0.20 0.40 -11 3 0 0.00 0.90 11 -3 0 -0.60 0.80 -11 2 0 0.90 1.20 -11 2 0 0.20 0.60 -11 2 0 -0.30 1.10 -11 2 0 0.60 0.80 11 -2 0 1.20 1.00 -11 1 0 -0.10 0.70 -11 1 0 -0.20 0.80 -11 1 0 0.60 1.20 -11 1 0 0.10 0.70 11 -1 0 -0.70 1.20 11 -1 0 -0.50 0.70 11 -1 0 -0.60 0.60 -11 -1 0 0.80 0.80 -11 -1 0 0.80 1.00 -11 -1 0 -0.10 0.80 11 1 0 0.60 0.70 11 1 0 -0.20 1.10 11 1 0 1.20 1.40 -11 -2 0 -0.20 0.80 -11 -2 0 -1.40 0.80 -11 -2 0 -1.70 0.70 11 2 0 0.70 1.30 11 2 0 0.30 1.50 11 2 0 -0.40 1.20 11 2 0 -0.60 0.60 11 3 0 1.60 1.50 11 3 0 0.10 1.20 11 3 0 0.30 1.20 11 4 0 0.20 1.40 11 4 0 0.20 1.10 11 4 0 -0.50 1.10 11 5 0 0.10 1.50 11 5 0 -1.00 1.00 11 5 0 -0.80 1.10 11 6 0 -1.10 1.10 11 6 0 -0.60 1.70 11 6 0 1.90 1.50 11 7 0 -0.20 1.40 11 7 0 1.10 1.60 -12 7 0 25.20 4.50 -12 7 0 23.80 4.20 -12 6 0 23.70 4.00 -12 6 0 24.50 4.20 -12 5 0 114.29 7.60 -12 5 0 106.79 7.10 -12 4 0 18.40 3.40 -12 4 0 31.20 4.80 -12 3 0 70.49 3.00 -12 3 0 59.89 2.50 -12 2 0 459.75 16.70 -12 2 0 456.05 16.00 -12 2 0 448.96 12.40 -12 2 0 441.66 13.30 12 -2 0 439.96 14.30 -12 1 0 56.39 5.90 -12 1 0 50.19 3.20 -12 1 0 45.80 4.90 -12 1 0 39.20 3.80 12 -1 0 46.30 4.40 12 -1 0 50.49 3.70 -12 0 0 227.98 9.10 -12 0 0 208.38 8.00 12 0 0 211.18 8.10 12 0 0 223.08 11.20 12 0 0 233.88 9.00 12 0 0 223.48 10.90 -12 -1 0 44.90 3.40 -12 -1 0 47.90 4.50 12 1 0 53.49 5.10 12 1 0 51.29 3.20 12 1 0 42.70 5.50 12 1 0 48.60 6.20 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1.50 2.00 13 3 0 0.20 1.80 13 4 0 1.50 1.70 13 4 0 1.60 2.00 13 4 0 0.50 1.70 13 5 0 0.70 1.70 13 5 0 -0.70 1.30 13 6 0 0.30 1.80 13 6 0 1.60 1.80 -14 6 0 2.30 2.00 -14 6 0 0.00 1.80 -14 5 0 22.30 4.20 -14 5 0 23.30 4.80 -14 4 0 15.80 3.60 -14 4 0 12.50 3.50 -14 3 0 1.00 2.00 -14 3 0 3.80 0.80 -14 3 0 4.40 2.00 -14 3 0 4.00 1.00 14 -3 0 3.00 1.60 -14 2 0 0.10 1.50 -14 2 0 -0.40 1.40 -14 2 0 1.00 1.00 -14 2 0 1.60 0.90 14 -2 0 1.10 1.30 -14 1 0 380.16 13.00 -14 1 0 386.76 11.90 14 -1 0 366.96 12.80 -14 0 0 19.20 2.60 14 0 0 20.20 2.70 -14 -1 0 346.17 12.20 -14 -1 0 378.26 13.70 14 1 0 359.06 13.80 14 1 0 381.96 18.30 14 1 0 384.76 11.90 14 1 0 378.66 16.50 -14 -2 0 1.20 1.20 -14 -2 0 0.10 1.30 14 2 0 1.50 2.00 14 2 0 2.30 2.10 14 2 0 0.70 1.60 14 2 0 0.20 0.80 14 3 0 2.70 2.10 14 3 0 5.10 2.50 14 3 0 5.50 2.50 14 4 0 10.80 3.10 14 4 0 11.90 3.40 14 4 0 11.60 3.70 14 5 0 35.00 5.90 14 5 0 21.80 4.60 14 6 0 0.10 2.00 14 6 0 1.90 2.10 -15 5 0 -0.30 1.80 -15 5 0 0.90 1.80 -15 4 0 -0.20 1.70 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8.50 2.30 2 5 3 12.00 1.50 2 5 3 10.80 1.60 2 5 3 10.80 1.50 -2 -5 -3 12.60 2.30 2 4 3 84.69 3.70 2 4 3 90.79 3.90 2 4 3 86.59 3.50 2 4 3 88.59 3.50 -2 -4 -3 89.59 4.70 2 3 3 53.59 2.70 2 3 3 54.59 2.80 2 3 3 56.39 2.60 2 3 3 55.29 2.50 -2 -3 -3 54.29 3.20 2 2 3 312.77 9.00 2 2 3 307.27 8.70 2 2 3 302.47 8.20 2 2 3 302.77 8.70 -2 -2 -3 308.67 9.00 2 1 3 2140.59 48.10 2 1 3 2183.08 48.00 2 1 3 2154.58 47.50 2 1 3 1886.91 47.10 2 1 3 2111.29 48.10 2 1 3 2111.69 47.60 -2 -1 -3 2022.90 47.30 -2 -1 -3 2013.80 50.79 -2 -1 -3 2102.39 47.50 -2 -1 -3 2129.09 47.60 2 0 3 0.10 0.20 2 0 3 0.30 0.40 2 0 3 0.20 0.20 2 0 3 0.00 0.30 -2 0 -3 0.30 0.30 -2 0 -3 0.20 0.30 -2 0 -3 0.10 0.20 -2 0 -3 0.70 0.30 -2 0 -3 -0.30 0.30 -2 0 -3 -0.40 0.20 2 -1 3 2135.49 47.40 2 -1 3 2169.38 46.70 2 -1 3 2154.48 46.80 2 -1 3 2052.39 46.60 -2 1 -3 2137.69 47.40 -2 1 -3 2013.50 48.10 -2 1 -3 1933.11 47.40 -2 1 -3 1953.40 47.30 -2 1 -3 2082.49 47.20 -2 1 -3 2108.09 47.30 -2 2 -3 305.07 8.00 -2 2 -3 312.67 8.20 -2 2 -3 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22.70 0.90 1 5 -4 20.60 1.00 -1 -6 4 20.40 2.80 1 6 -4 20.40 3.40 1 6 -4 13.70 2.50 -1 -7 4 120.79 6.50 1 7 -4 114.09 7.40 1 7 -4 119.29 6.70 -1 -8 4 16.70 3.10 1 8 -4 13.30 3.40 -2 9 4 37.90 3.60 -2 9 4 30.60 3.00 -2 8 4 8.80 1.70 -2 8 4 11.00 1.90 -2 7 4 -0.60 0.50 -2 7 4 0.10 0.60 2 -7 -4 0.20 1.10 -2 6 4 8.50 1.60 -2 6 4 8.00 1.70 -2 6 4 6.60 1.40 2 -6 -4 3.90 1.70 -2 5 4 0.90 0.80 -2 5 4 1.00 0.70 -2 5 4 0.40 0.50 -2 5 4 0.00 0.50 -2 5 4 -0.40 0.50 2 -5 -4 1.20 1.00 -2 4 4 250.07 7.50 -2 4 4 227.28 7.60 -2 4 4 239.48 6.70 -2 4 4 232.38 7.60 2 -4 -4 229.38 8.80 -2 3 4 29.40 1.20 -2 3 4 34.20 2.20 -2 3 4 32.00 3.00 -2 3 4 28.50 1.90 -2 2 4 1137.89 27.20 -2 2 4 1128.69 27.40 -2 2 4 1150.28 25.50 -2 2 4 1143.39 25.50 2 -2 -4 1144.29 27.50 2 -2 -4 1130.89 26.40 -2 1 4 73.49 2.40 -2 1 4 72.89 3.00 -2 1 4 73.89 2.70 -2 1 4 73.09 3.10 2 -1 -4 73.69 2.50 2 -1 -4 77.59 2.80 -2 0 4 86.19 2.70 -2 0 4 91.09 3.80 -2 0 4 88.29 3.10 -2 0 4 88.49 3.30 2 0 -4 85.19 2.90 2 0 -4 85.39 3.50 2 0 -4 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0.90 3 -6 -4 0.70 1.30 -3 5 4 16.10 1.90 -3 5 4 16.80 2.20 -3 5 4 16.60 2.00 -3 5 4 18.40 2.20 -3 5 4 13.90 1.60 3 -5 -4 19.30 2.90 -3 4 4 4.00 0.70 -3 4 4 3.60 1.00 -3 4 4 3.80 1.00 -3 4 4 4.70 1.10 -3 3 4 169.48 5.90 -3 3 4 168.18 4.60 -3 3 4 177.88 6.20 3 -3 -4 170.38 5.40 -3 2 4 134.29 3.70 -3 2 4 137.19 3.70 -3 2 4 139.09 3.90 -3 2 4 132.19 5.00 -3 2 4 133.89 3.60 -3 2 4 143.59 5.00 3 -2 -4 141.29 4.40 3 -2 -4 131.89 5.10 -3 1 4 99.59 3.80 -3 1 4 91.99 3.80 -3 1 4 95.39 3.40 -3 1 4 91.49 3.00 3 -1 -4 87.39 3.30 3 -1 -4 89.79 4.00 3 -1 -4 96.99 4.70 3 -1 -4 94.89 3.10 -3 0 4 804.52 19.40 -3 0 4 812.82 19.80 -3 0 4 810.22 19.40 -3 0 4 774.62 18.90 -3 0 4 803.52 19.90 3 0 -4 796.52 19.80 3 0 -4 829.12 20.40 3 0 -4 814.22 19.00 3 0 -4 792.62 19.20 -3 -1 4 92.49 3.80 -3 -1 4 94.49 3.20 -3 -1 4 91.39 2.90 -3 -1 4 87.59 3.40 3 1 -4 90.69 2.70 3 1 -4 87.79 3.40 3 1 -4 93.19 2.60 3 1 -4 90.09 4.10 3 1 -4 91.49 3.70 3 1 -4 92.29 2.60 3 1 -4 87.69 3.80 3 1 -4 95.39 2.70 -3 -2 4 137.09 3.30 -3 -2 4 126.39 3.30 3 2 -4 129.69 4.40 3 2 -4 132.59 4.50 3 2 -4 134.89 4.80 3 2 -4 131.09 4.30 3 2 -4 133.09 5.30 3 2 -4 136.29 5.70 3 3 -4 164.18 6.60 3 3 -4 161.98 5.10 3 3 -4 167.48 7.10 3 3 -4 158.58 5.20 3 3 -4 165.18 5.50 3 3 -4 171.38 5.60 -3 -4 4 3.40 1.00 3 4 -4 5.00 1.00 3 4 -4 3.70 1.40 3 4 -4 3.00 0.70 3 4 -4 4.80 0.80 3 4 -4 5.30 1.50 -3 -5 4 17.20 2.40 3 5 -4 16.00 3.00 3 5 -4 18.90 1.80 3 5 -4 17.20 1.30 3 5 -4 17.00 1.30 3 5 -4 14.50 2.60 -3 -6 4 -0.30 0.80 3 6 -4 0.20 1.10 3 6 -4 0.10 0.40 3 6 -4 0.60 0.40 3 6 -4 0.50 1.30 3 6 -4 -0.40 0.40 3 6 -4 0.10 0.40 -3 -7 4 0.80 1.20 3 7 -4 1.20 0.50 3 7 -4 0.70 0.60 3 7 -4 1.00 1.50 3 7 -4 1.60 1.60 -3 -8 4 88.39 6.50 3 8 -4 95.19 6.80 3 8 -4 100.59 3.80 3 8 -4 93.59 7.40 -4 9 4 13.20 2.50 -4 9 4 12.30 2.30 -4 8 4 2.90 1.20 -4 8 4 2.60 1.30 -4 7 4 56.29 3.90 -4 7 4 61.09 3.90 4 -7 -4 60.79 6.10 -4 6 4 144.69 6.20 -4 6 4 147.39 6.40 4 -6 -4 149.99 7.90 -4 5 4 161.48 6.70 -4 5 4 172.28 5.70 -4 5 4 178.98 6.70 -4 4 4 3.10 1.00 -4 4 4 2.70 0.60 -4 4 4 2.00 0.60 -4 4 4 2.90 0.90 -4 4 4 1.40 0.90 -4 3 4 397.16 9.80 -4 3 4 377.76 11.50 -4 3 4 384.06 11.30 4 -3 -4 393.16 10.40 -4 2 4 17.70 1.20 -4 2 4 17.50 1.10 -4 2 4 15.80 2.00 -4 2 4 17.00 1.00 -4 2 4 15.40 1.90 4 -2 -4 15.20 2.00 4 -2 -4 14.60 1.50 -4 1 4 1483.35 35.30 -4 1 4 1479.05 34.70 -4 1 4 1492.65 33.90 -4 1 4 1473.95 33.90 -4 1 4 1465.65 35.50 4 -1 -4 1448.96 35.90 4 -1 -4 1509.45 34.60 4 -1 -4 1456.95 34.60 -4 0 4 69.99 3.30 -4 0 4 79.29 3.20 -4 0 4 74.69 2.80 -4 0 4 69.29 3.40 -4 0 4 77.69 3.10 4 0 -4 72.99 3.00 4 0 -4 68.99 3.70 4 0 -4 71.79 3.70 4 0 -4 75.09 2.80 -4 -1 4 1460.45 33.70 -4 -1 4 1471.25 34.20 -4 -1 4 1519.25 36.10 -4 -1 4 1396.06 34.50 4 1 -4 1456.25 35.00 4 1 -4 1469.85 35.50 4 1 -4 1453.95 35.80 4 1 -4 1456.25 33.40 4 1 -4 1473.65 33.40 4 1 -4 1491.85 35.40 4 1 -4 1459.85 34.70 -4 -2 4 16.30 1.00 4 2 -4 17.90 1.70 4 2 -4 14.20 2.10 4 2 -4 15.60 1.80 4 2 -4 20.20 1.90 4 2 -4 15.60 2.10 4 2 -4 16.20 2.00 4 3 -4 394.56 11.40 4 3 -4 380.66 12.30 4 3 -4 385.76 10.80 4 3 -4 397.76 13.00 4 3 -4 388.56 10.60 4 3 -4 386.66 11.00 4 4 -4 3.30 1.40 4 4 -4 2.20 0.70 4 4 -4 2.50 0.80 4 4 -4 2.20 0.80 4 4 -4 2.20 0.70 4 4 -4 1.80 1.20 4 5 -4 163.88 5.50 4 5 -4 170.68 5.70 4 5 -4 185.18 8.80 4 5 -4 172.08 6.20 4 5 -4 164.08 5.90 4 5 -4 175.98 8.20 4 6 -4 155.18 8.10 4 6 -4 140.49 8.30 4 6 -4 144.09 5.00 4 6 -4 150.48 5.60 4 6 -4 148.39 5.10 4 6 -4 153.58 5.60 -4 -7 4 68.19 4.90 4 7 -4 63.29 2.80 4 7 -4 64.69 3.50 4 7 -4 62.89 6.90 4 7 -4 80.09 6.00 4 7 -4 65.09 3.00 4 8 -4 1.80 0.80 4 8 -4 0.80 1.60 4 9 -4 13.50 1.70 -5 9 4 40.50 4.20 -5 9 4 26.80 3.60 -5 8 4 62.49 4.40 -5 8 4 62.59 4.50 -5 7 4 43.40 4.10 -5 7 4 53.09 3.90 5 -7 -4 42.70 5.30 -5 6 4 100.19 5.20 -5 6 4 96.59 5.30 -5 5 4 18.20 2.40 -5 5 4 13.40 2.20 -5 4 4 2.60 1.10 -5 4 4 2.80 0.70 -5 4 4 0.50 0.70 -5 4 4 2.00 0.90 -5 3 4 11.60 1.80 -5 3 4 7.70 1.60 -5 3 4 9.80 1.80 5 -3 -4 8.40 1.30 5 -3 -4 8.50 1.60 -5 2 4 14.90 2.00 -5 2 4 12.00 0.90 -5 2 4 12.90 1.90 -5 2 4 10.90 0.70 -5 2 4 8.30 1.60 -5 2 4 10.90 1.30 5 -2 -4 11.10 1.50 5 -2 -4 10.70 1.90 -5 1 4 134.69 4.30 -5 1 4 137.69 4.40 -5 1 4 147.29 5.70 -5 1 4 149.49 5.60 -5 1 4 133.69 5.00 5 -1 -4 135.59 4.90 5 -1 -4 134.89 6.00 -5 0 4 9.80 1.60 -5 0 4 7.50 1.30 -5 0 4 6.70 1.30 -5 0 4 7.50 1.00 -5 0 4 9.30 1.30 5 0 -4 5.40 1.40 5 0 -4 8.00 1.20 5 0 -4 7.40 1.10 5 0 -4 6.60 1.10 5 0 -4 8.60 1.70 -5 -1 4 135.29 4.70 -5 -1 4 134.79 5.00 -5 -1 4 138.69 4.40 5 1 -4 134.79 4.10 5 1 -4 137.39 5.70 5 1 -4 129.19 5.00 5 1 -4 125.69 5.60 5 1 -4 108.59 3.80 5 1 -4 141.79 5.30 -5 -2 4 9.80 1.20 -5 -2 4 10.50 1.10 -5 -2 4 12.10 1.50 5 2 -4 9.90 1.70 5 2 -4 12.90 1.90 5 2 -4 8.10 1.60 -5 -3 4 11.10 1.00 5 3 -4 5.50 1.70 5 3 -4 8.90 1.60 5 3 -4 9.20 1.90 5 3 -4 8.60 1.60 5 3 -4 8.40 1.40 5 3 -4 9.00 1.40 5 4 -4 3.10 0.90 5 4 -4 3.10 1.10 5 4 -4 1.80 1.20 5 4 -4 1.90 1.20 5 4 -4 3.10 1.00 5 4 -4 3.00 0.90 5 5 -4 13.50 1.80 5 5 -4 11.80 1.60 5 5 -4 12.00 2.60 5 5 -4 12.10 1.90 5 5 -4 13.50 2.00 5 5 -4 15.30 3.10 5 6 -4 103.59 6.70 5 6 -4 102.59 4.90 5 6 -4 95.39 4.70 5 6 -4 100.99 7.10 5 7 -4 39.30 5.20 5 7 -4 46.70 3.00 5 7 -4 49.50 3.30 5 8 -4 57.29 6.70 5 8 -4 63.99 2.90 5 8 -4 65.29 3.90 5 9 -4 35.40 3.20 -6 9 4 1.80 1.40 -6 9 4 5.20 1.90 -6 8 4 2.10 1.40 -6 8 4 4.60 1.80 -6 7 4 51.79 4.00 -6 7 4 46.40 4.50 -6 6 4 24.30 3.20 -6 6 4 22.10 2.90 -6 5 4 109.19 5.80 -6 5 4 116.19 5.70 -6 4 4 39.10 3.10 -6 4 4 45.30 3.40 -6 4 4 46.20 2.50 -6 3 4 71.89 4.50 -6 3 4 67.99 4.10 -6 3 4 76.29 4.20 6 -3 -4 69.39 4.10 6 -3 -4 67.59 3.40 -6 2 4 19.90 1.90 -6 2 4 18.30 2.30 -6 2 4 16.10 2.30 -6 2 4 14.60 1.10 -6 2 4 16.40 1.60 6 -2 -4 18.30 2.00 6 -2 -4 12.30 2.20 -6 1 4 296.57 9.80 -6 1 4 304.67 8.30 -6 1 4 290.97 9.90 -6 1 4 302.27 9.20 6 -1 -4 313.97 10.60 6 -1 -4 294.37 10.50 6 -1 -4 308.67 9.10 -6 0 4 86.69 4.30 -6 0 4 77.79 4.00 -6 0 4 84.39 3.30 -6 0 4 77.79 3.80 6 0 -4 76.69 3.50 6 0 -4 75.79 4.40 6 0 -4 74.49 3.40 6 0 -4 85.29 3.40 6 0 -4 79.89 4.60 -6 -1 4 285.67 8.30 -6 -1 4 292.77 9.20 -6 -1 4 283.57 8.80 6 1 -4 290.67 10.20 6 1 -4 290.17 7.90 6 1 -4 289.67 8.00 6 1 -4 294.97 9.40 6 1 -4 308.07 10.20 -6 -2 4 16.60 1.80 -6 -2 4 16.40 1.60 -6 -2 4 15.10 1.80 6 2 -4 15.00 2.30 6 2 -4 18.70 2.60 6 2 -4 15.00 2.20 6 2 -4 19.00 2.20 -6 -3 4 72.09 2.80 6 3 -4 67.49 3.70 6 3 -4 69.39 3.80 6 3 -4 72.69 4.20 6 3 -4 74.49 4.60 6 3 -4 67.69 4.20 6 4 -4 44.50 2.90 6 4 -4 38.20 3.70 6 4 -4 39.20 2.80 6 4 -4 30.80 3.80 6 4 -4 37.90 3.60 6 5 -4 117.29 5.60 6 5 -4 101.69 6.50 6 5 -4 108.89 5.50 6 6 -4 35.70 4.70 6 6 -4 29.70 3.30 6 6 -4 27.40 3.10 6 7 -4 47.40 3.40 6 7 -4 58.09 4.00 6 7 -4 48.90 5.90 6 8 -4 3.80 1.50 6 8 -4 5.70 1.40 6 9 -4 1.50 1.20 -7 8 4 69.89 5.20 -7 8 4 62.79 5.70 -7 7 4 0.70 1.10 -7 7 4 -0.10 1.00 -7 6 4 0.50 1.00 -7 6 4 1.10 1.10 -7 5 4 191.28 8.40 -7 5 4 183.98 8.00 -7 4 4 3.00 1.30 -7 4 4 5.70 1.70 -7 3 4 75.89 2.40 -7 3 4 70.19 4.40 -7 3 4 78.19 2.40 -7 3 4 74.69 4.60 -7 3 4 76.29 2.10 -7 3 4 71.99 2.10 7 -3 -4 75.69 3.80 -7 2 4 497.55 14.70 -7 2 4 498.35 15.00 -7 2 4 464.65 13.10 -7 2 4 473.15 12.80 -7 2 4 487.55 12.30 7 -2 -4 495.75 15.40 7 -2 -4 485.85 15.50 7 -2 -4 480.65 13.60 -7 1 4 16.30 2.40 -7 1 4 17.80 2.40 -7 1 4 25.50 2.60 -7 1 4 16.90 1.60 7 -1 -4 20.70 2.20 7 -1 -4 18.20 2.70 7 -1 -4 23.60 3.20 -7 0 4 167.98 6.60 -7 0 4 168.68 6.30 -7 0 4 157.88 5.50 -7 0 4 161.48 6.80 7 0 -4 161.18 5.80 7 0 -4 161.38 5.50 7 0 -4 165.08 7.40 7 0 -4 160.08 5.80 7 0 -4 151.38 7.10 -7 -1 4 25.30 2.80 -7 -1 4 20.50 2.40 -7 -1 4 20.30 2.30 -7 -1 4 17.30 1.80 7 1 -4 16.90 2.60 7 1 -4 16.70 1.60 7 1 -4 21.00 2.40 7 1 -4 20.50 1.50 7 1 -4 18.00 2.70 -7 -2 4 492.15 13.80 -7 -2 4 491.15 13.60 -7 -2 4 485.65 13.00 7 2 -4 474.85 14.30 7 2 -4 475.65 15.40 7 2 -4 504.35 15.40 7 2 -4 495.35 15.00 -7 -3 4 79.09 3.60 -7 -3 4 77.79 3.30 7 3 -4 71.59 4.80 7 3 -4 72.19 4.60 7 3 -4 77.59 4.80 7 3 -4 74.89 4.10 7 4 -4 3.80 1.40 7 4 -4 3.90 1.70 7 4 -4 5.50 1.60 7 5 -4 187.68 9.30 7 5 -4 173.58 7.80 7 5 -4 179.48 8.00 7 6 -4 0.50 0.90 7 6 -4 0.20 0.90 7 6 -4 0.30 1.30 7 7 -4 0.60 1.50 7 7 -4 0.60 1.10 7 7 -4 0.30 0.90 7 8 -4 69.89 4.90 7 8 -4 73.99 4.40 -8 8 4 -1.20 1.10 -8 8 4 -0.50 1.20 -8 7 4 6.20 2.00 -8 7 4 9.90 2.40 -8 6 4 64.99 5.00 -8 6 4 61.89 4.70 -8 5 4 39.80 4.30 -8 5 4 35.90 4.10 -8 4 4 20.90 3.30 -8 4 4 25.00 3.40 -8 3 4 15.00 1.20 -8 3 4 16.00 1.00 -8 3 4 13.20 1.00 -8 3 4 12.00 2.30 -8 3 4 15.70 1.10 -8 3 4 12.70 2.20 8 -3 -4 19.60 2.40 -8 2 4 671.13 17.60 -8 2 4 690.33 17.00 -8 2 4 678.73 18.00 -8 2 4 690.03 20.10 -8 2 4 686.73 19.80 8 -2 -4 685.73 18.50 8 -2 -4 675.23 20.60 8 -2 -4 685.33 20.40 -8 1 4 39.80 4.10 -8 1 4 36.70 2.80 -8 1 4 54.99 3.70 -8 1 4 41.50 2.40 8 -1 -4 49.60 4.80 8 -1 -4 40.80 2.30 8 -1 -4 41.40 2.90 8 -1 -4 43.90 4.70 -8 0 4 765.82 21.10 -8 0 4 761.12 20.60 -8 0 4 756.02 19.40 -8 0 4 768.82 21.60 8 0 -4 791.62 22.50 8 0 -4 741.23 22.40 8 0 -4 779.52 19.90 8 0 -4 765.62 20.00 -8 -1 4 41.50 3.10 -8 -1 4 42.40 4.10 -8 -1 4 39.80 2.60 -8 -1 4 47.10 3.20 8 1 -4 42.40 2.40 8 1 -4 43.40 4.40 8 1 -4 47.30 4.90 8 1 -4 40.60 2.30 8 1 -4 46.40 3.30 -8 -2 4 691.63 18.50 -8 -2 4 674.93 18.40 -8 -2 4 666.23 17.60 8 2 -4 675.43 16.10 8 2 -4 695.13 15.80 8 2 -4 664.63 20.40 8 2 -4 664.53 15.80 8 2 -4 695.03 20.40 8 2 -4 657.23 19.60 8 2 -4 668.53 15.90 -8 -3 4 14.60 1.80 8 3 -4 14.70 2.70 8 3 -4 11.40 2.40 8 3 -4 10.80 2.20 8 4 -4 22.50 3.30 8 4 -4 25.60 3.50 8 4 -4 19.50 3.20 8 5 -4 38.50 4.30 8 5 -4 37.50 4.20 8 5 -4 39.10 4.90 8 6 -4 65.29 4.90 8 6 -4 64.59 6.80 8 6 -4 66.09 4.90 8 7 -4 8.70 2.20 8 7 -4 8.90 2.20 8 7 -4 4.90 2.40 8 8 -4 1.20 1.30 8 8 -4 0.40 1.10 -9 8 4 11.60 2.90 -9 8 4 10.60 2.90 -9 7 4 0.30 1.20 -9 7 4 -1.30 0.90 -9 6 4 156.78 8.20 -9 6 4 133.19 7.50 -9 5 4 107.49 6.40 -9 5 4 92.29 6.10 -9 4 4 92.99 5.80 -9 4 4 92.59 5.90 -9 3 4 145.39 7.10 -9 3 4 134.29 4.60 -9 3 4 131.39 4.10 -9 3 4 140.09 7.20 9 -3 -4 133.39 6.00 -9 2 4 276.47 10.50 -9 2 4 276.97 10.80 -9 2 4 280.37 8.10 -9 2 4 261.27 8.90 9 -2 -4 264.67 10.90 9 -2 -4 284.17 9.50 -9 1 4 24.90 2.90 -9 1 4 21.40 2.60 -9 1 4 24.40 3.30 -9 1 4 20.30 2.80 -9 1 4 25.70 2.40 9 -1 -4 16.10 1.80 9 -1 -4 23.60 3.50 9 -1 -4 25.30 2.90 9 -1 -4 19.80 3.40 -9 0 4 32.40 3.70 -9 0 4 37.00 3.70 -9 0 4 33.00 3.40 -9 0 4 32.20 2.40 9 0 -4 27.80 2.70 9 0 -4 32.70 2.60 9 0 -4 38.30 4.40 9 0 -4 43.30 4.90 -9 -1 4 23.50 2.90 -9 -1 4 23.20 2.90 -9 -1 4 22.00 3.10 -9 -1 4 21.40 2.20 9 1 -4 18.20 3.00 9 1 -4 22.10 2.80 9 1 -4 26.10 1.90 9 1 -4 25.50 3.80 9 1 -4 22.10 2.20 -9 -2 4 271.27 9.60 -9 -2 4 268.37 8.80 9 2 -4 270.07 11.30 9 2 -4 284.47 10.60 9 2 -4 268.57 7.20 9 2 -4 270.47 7.30 9 2 -4 270.57 11.20 9 2 -4 277.57 8.50 9 2 -4 280.27 7.30 -9 -3 4 134.09 6.00 9 3 -4 139.19 7.60 9 3 -4 144.89 7.60 9 3 -4 138.79 7.30 9 4 -4 96.79 6.20 9 4 -4 83.19 5.80 9 4 -4 88.19 6.10 9 5 -4 86.59 6.00 9 5 -4 89.59 6.60 9 5 -4 99.99 6.30 9 6 -4 145.69 9.00 9 6 -4 148.79 8.00 9 6 -4 158.88 8.30 9 7 -4 0.40 1.20 9 7 -4 -1.00 1.10 9 8 -4 11.60 2.80 9 8 -4 10.30 2.40 -10 8 4 30.70 4.80 -10 7 4 19.40 3.60 -10 7 4 19.10 3.60 -10 6 4 5.60 2.10 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5.90 1 -1 -25 69.09 5.10 -1 0 25 0.60 1.60 1 0 -25 -1.90 0.90 -1 -1 25 59.99 6.40 1 2 -25 7.40 2.90 1 2 -25 18.30 4.30 1 3 -25 28.60 5.50 1 3 -25 39.60 6.10 2 -3 -25 92.29 6.60 -2 2 25 0.60 1.50 2 -2 -25 -0.30 1.20 -2 1 25 0.30 1.60 2 -1 -25 0.20 1.20 -2 0 25 0.40 1.50 2 0 -25 0.50 1.10 -2 -1 25 -0.70 1.50 2 2 -25 -0.40 1.80 2 2 -25 -0.50 1.60 -3 2 25 45.90 5.40 3 -2 -25 46.70 5.20 -3 1 25 4.40 2.20 3 -1 -25 4.60 2.00 -3 0 25 0.90 1.70 3 0 -25 0.00 1.00 -3 -1 25 5.00 2.50 3 2 -25 38.30 6.00 3 2 -25 48.00 7.10 -4 2 25 14.80 3.10 4 -2 -25 15.90 3.10 -4 1 25 24.20 4.30 4 -1 -25 16.20 2.90 -4 0 25 0.60 1.70 4 0 -25 0.60 1.10 -4 -1 25 17.80 3.80 4 2 -25 20.40 4.80 4 2 -25 18.50 4.50 -5 1 25 55.89 6.10 5 -1 -25 64.49 5.00 -5 0 25 0.70 1.80 5 0 -25 1.00 1.20 -5 -1 25 61.49 6.60 6 0 -25 0.80 1.20 3 0 26 62.69 6.60 -3 0 -26 63.39 4.40 2 1 26 6.70 2.50 -2 -1 -26 15.80 3.00 2 0 26 3.00 2.10 -2 0 -26 7.90 1.90 2 -1 26 22.40 4.10 -2 1 -26 10.20 3.40 1 1 26 11.50 3.00 -1 -1 -26 17.00 3.00 1 0 26 0.80 1.70 -1 0 -26 4.90 1.60 1 -1 26 15.00 3.50 0 1 26 -2.20 1.10 0 -1 -26 -0.40 1.30 0 0 26 5.00 2.30 0 0 -26 7.40 1.90 0 -1 26 -1.50 1.50 -1 1 26 13.20 3.20 1 -1 -26 16.80 3.00 -1 0 26 3.50 2.20 1 0 -26 4.30 1.60 -1 -1 26 16.60 3.70 -2 1 26 14.20 3.30 2 -1 -26 15.40 3.00 -2 0 26 3.60 2.10 2 0 -26 2.40 1.40 -2 -1 26 22.40 4.10 -3 0 26 67.09 7.00 3 0 -26 61.39 4.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' ; _shelx_hkl_checksum 91541 _shelx_res_file ; TITL test_a.res in Pbca test.res created by SHELXL-2018/3 at 21:52:22 on 08-Feb-2023 REM Old TITL test in Pbca REM SHELXT solution in Pbca: R1 0.106, Rweak 0.001, Alpha 0.013 REM 0.593 for 326 systematic absences, Orientation as input REM Formula found by SHELXT: C13 N2 O CELL 0.71073 13.7925 7.2652 19.7956 90 90 90 ZERR 8 0.0003 0.0001 0.0004 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 104 80 16 8 L.S. 20 PLAN 5 SIZE 0.188 0.329 0.368 TEMP -80 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.040100 1.386600 FVAR 0.47556 O1 4 0.455680 0.033818 0.590302 11.00000 0.02758 0.01637 = 0.01677 -0.00020 0.00062 0.00506 N1 3 0.388059 0.329743 0.589597 11.00000 0.01732 0.01503 = 0.01447 -0.00215 0.00049 0.00213 N3 3 0.431993 0.205140 0.492423 11.00000 0.01879 0.01567 = 0.01422 -0.00217 0.00042 0.00283 AFIX 43 H3 2 0.452728 0.125653 0.462151 11.00000 -1.20000 AFIX 0 C7A 1 0.370194 0.460384 0.539143 11.00000 0.01219 0.01723 = 0.01562 -0.00082 -0.00066 -0.00125 C2 1 0.428847 0.173582 0.560543 11.00000 0.01571 0.01681 = 0.01609 -0.00268 0.00036 0.00035 C8 1 0.374842 0.357721 0.660311 11.00000 0.02152 0.01370 = 0.01405 -0.00197 0.00234 -0.00142 C3A 1 0.397832 0.380313 0.477905 11.00000 0.01190 0.01598 = 0.01781 -0.00251 -0.00014 0.00007 C7 1 0.336063 0.639059 0.542148 11.00000 0.01485 0.01771 = 0.02026 -0.00352 0.00122 0.00055 AFIX 43 H7 2 0.319418 0.694844 0.583974 11.00000 -1.20000 AFIX 0 C4 1 0.388125 0.473036 0.417479 11.00000 0.01662 0.02075 = 0.01608 -0.00105 0.00044 0.00016 AFIX 43 H4 2 0.405896 0.417587 0.375818 11.00000 -1.20000 AFIX 0 C5 1 0.351165 0.651458 0.420072 11.00000 0.01667 0.02150 = 0.02018 0.00391 -0.00064 -0.00009 AFIX 43 H5 2 0.342230 0.718091 0.379252 11.00000 -1.20000 AFIX 0 C9 1 0.449155 0.314739 0.705120 11.00000 0.02189 0.01991 = 0.01758 -0.00002 0.00049 -0.00225 AFIX 43 H9 2 0.507674 0.261337 0.689104 11.00000 -1.20000 AFIX 0 C13 1 0.288370 0.433114 0.683601 11.00000 0.02414 0.01616 = 0.02055 -0.00137 0.00306 0.00095 AFIX 43 H13 2 0.237403 0.460514 0.652926 11.00000 -1.20000 AFIX 0 C6 1 0.327070 0.734007 0.481318 11.00000 0.01510 0.01663 = 0.02577 0.00058 0.00039 0.00110 AFIX 43 H6 2 0.304090 0.857272 0.481620 11.00000 -1.20000 AFIX 0 C12 1 0.277284 0.467982 0.752270 11.00000 0.03533 0.01799 = 0.02368 -0.00237 0.01167 0.00245 AFIX 43 H12 2 0.218579 0.520089 0.768528 11.00000 -1.20000 AFIX 0 C11 1 0.351278 0.427193 0.797009 11.00000 0.04595 0.01885 = 0.01560 -0.00306 0.00582 -0.00473 AFIX 43 H11 2 0.343401 0.451607 0.843835 11.00000 -1.20000 AFIX 0 C10 1 0.436969 0.350635 0.773460 11.00000 0.03396 0.02305 = 0.01661 0.00126 -0.00282 -0.00660 AFIX 43 H10 2 0.487637 0.322592 0.804296 11.00000 -1.20000 AFIX 0 HKLF 4 REM test_a.res in Pbca REM wR2 = 0.0989, GooF = S = 1.018, Restrained GooF = 1.018 for all data REM R1 = 0.0391 for 2203 Fo > 4sig(Fo) and 0.0438 for all 2479 data REM 145 parameters refined using 0 restraints END WGHT 0.0407 1.3386 REM Highest difference peak 0.245, deepest hole -0.375, 1-sigma level 0.054 Q1 1 0.4348 0.3190 0.7401 11.00000 0.05 0.25 Q2 1 0.3725 0.5668 0.4199 11.00000 0.05 0.24 Q3 1 0.3217 0.3568 0.6754 11.00000 0.05 0.23 Q4 1 0.4169 0.3599 0.6829 11.00000 0.05 0.22 Q5 1 0.3833 0.3424 0.6240 11.00000 0.05 0.22 ; _shelx_res_checksum 35761 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, 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 0.45568(7) 0.03382(12) 0.59030(4) 0.0202(2) Uani d 1 . . N N1 0.38806(7) 0.32974(13) 0.58960(5) 0.0156(2) Uani d 1 . . N N3 0.43199(7) 0.20514(13) 0.49242(5) 0.0162(2) Uani d 1 . . H H3 0.452728 0.125653 0.462151 0.019 Uiso calc 1 . . C C7A 0.37019(8) 0.46038(16) 0.53914(6) 0.0150(2) Uani d 1 . . C C2 0.42885(8) 0.17358(16) 0.56054(6) 0.0162(2) Uani d 1 . . C C8 0.37484(8) 0.35772(16) 0.66031(6) 0.0164(2) Uani d 1 . . C C3A 0.39783(8) 0.38031(16) 0.47791(6) 0.0152(2) Uani d 1 . . C C7 0.33606(8) 0.63906(16) 0.54215(6) 0.0176(2) Uani d 1 . . H H7 0.319418 0.694844 0.583974 0.021 Uiso calc 1 . . C C4 0.38813(8) 0.47304(17) 0.41748(6) 0.0178(2) Uani d 1 . . H H4 0.405896 0.417587 0.375818 0.021 Uiso calc 1 . . C C5 0.35117(8) 0.65146(17) 0.42007(6) 0.0195(2) Uani d 1 . . H H5 0.342230 0.718091 0.379252 0.023 Uiso calc 1 . . C C9 0.44915(9) 0.31474(17) 0.70512(6) 0.0198(2) Uani d 1 . . H H9 0.507674 0.261337 0.689104 0.024 Uiso calc 1 . . C C13 0.28837(9) 0.43311(16) 0.68360(6) 0.0203(3) Uani d 1 . . H H13 0.237403 0.460514 0.652926 0.024 Uiso calc 1 . . C C6 0.32707(8) 0.73401(17) 0.48132(6) 0.0192(2) Uani d 1 . . H H6 0.304090 0.857272 0.481620 0.023 Uiso calc 1 . . C C12 0.27728(10) 0.46798(17) 0.75227(7) 0.0257(3) Uani d 1 . . H H12 0.218579 0.520089 0.768528 0.031 Uiso calc 1 . . C C11 0.35128(11) 0.42719(17) 0.79701(6) 0.0268(3) Uani d 1 . . H H11 0.343401 0.451607 0.843835 0.032 Uiso calc 1 . . C C10 0.43697(10) 0.35064(18) 0.77346(6) 0.0245(3) Uani d 1 . . H H10 0.487637 0.322592 0.804296 0.029 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 0.0276(5) 0.0164(4) 0.0168(4) 0.0051(3) 0.0006(3) -0.0002(3) N1 0.0173(4) 0.0150(4) 0.0145(4) 0.0021(4) 0.0005(3) -0.0022(4) N3 0.0188(5) 0.0157(5) 0.0142(4) 0.0028(4) 0.0004(4) -0.0022(4) C7A 0.0122(5) 0.0172(5) 0.0156(5) -0.0013(4) -0.0007(4) -0.0008(4) C2 0.0157(5) 0.0168(5) 0.0161(5) 0.0004(4) 0.0004(4) -0.0027(4) C8 0.0215(5) 0.0137(5) 0.0140(5) -0.0014(4) 0.0023(4) -0.0020(4) C3A 0.0119(5) 0.0160(5) 0.0178(5) 0.0001(4) -0.0001(4) -0.0025(4) C7 0.0148(5) 0.0177(5) 0.0203(5) 0.0006(4) 0.0012(4) -0.0035(4) C4 0.0166(5) 0.0208(6) 0.0161(5) 0.0002(4) 0.0004(4) -0.0011(4) C5 0.0167(5) 0.0215(6) 0.0202(6) -0.0001(5) -0.0006(4) 0.0039(5) C9 0.0219(6) 0.0199(5) 0.0176(5) -0.0022(5) 0.0005(4) 0.0000(4) C13 0.0241(6) 0.0162(5) 0.0205(6) 0.0009(5) 0.0031(5) -0.0014(4) C6 0.0151(5) 0.0166(5) 0.0258(6) 0.0011(4) 0.0004(4) 0.0006(5) C12 0.0353(7) 0.0180(6) 0.0237(6) 0.0025(5) 0.0117(5) -0.0024(5) C11 0.0460(8) 0.0188(6) 0.0156(5) -0.0047(6) 0.0058(5) -0.0031(5) C10 0.0340(7) 0.0230(6) 0.0166(6) -0.0066(5) -0.0028(5) 0.0013(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 C7A N1 C8 . . 125.54(10) ? C2 N1 C7A . . 109.23(9) ? C2 N1 C8 . . 125.02(10) ? C2 N3 H3 . . 124.8 ? C2 N3 C3A . . 110.31(9) ? C3A N3 H3 . . 124.8 ? C3A C7A N1 . . 106.78(10) ? C7 C7A N1 . . 131.77(11) ? C7 C7A C3A . . 121.41(11) ? O1 C2 N1 . . 126.63(11) ? O1 C2 N3 . . 126.89(11) ? N3 C2 N1 . . 106.48(10) ? C9 C8 N1 . . 119.98(10) ? C9 C8 C13 . . 120.59(11) ? C13 C8 N1 . . 119.41(10) ? N3 C3A C7A . . 107.15(10) ? C4 C3A N3 . . 131.35(11) ? C4 C3A C7A . . 121.50(11) ? C7A C7 H7 . . 121.4 ? C7A C7 C6 . . 117.27(11) ? C6 C7 H7 . . 121.4 ? C3A C4 H4 . . 121.4 ? C3A C4 C5 . . 117.24(11) ? C5 C4 H4 . . 121.4 ? C4 C5 H5 . . 119.3 ? C6 C5 C4 . . 121.32(11) ? C6 C5 H5 . . 119.3 ? C8 C9 H9 . . 120.3 ? C10 C9 C8 . . 119.35(12) ? C10 C9 H9 . . 120.3 ? C8 C13 H13 . . 120.3 ? C8 C13 C12 . . 119.33(12) ? C12 C13 H13 . . 120.3 ? C7 C6 H6 . . 119.4 ? C5 C6 C7 . . 121.19(11) ? C5 C6 H6 . . 119.4 ? C13 C12 H12 . . 119.8 ? C11 C12 C13 . . 120.36(12) ? C11 C12 H12 . . 119.8 ? C12 C11 H11 . . 120.0 ? C12 C11 C10 . . 119.96(12) ? C10 C11 H11 . . 120.0 ? C9 C10 H10 . . 119.8 ? C11 C10 C9 . . 120.41(12) ? C11 C10 H10 . . 119.8 ? 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 C2 . 1.2309(14) ? N1 C7A . 1.3997(15) ? N1 C2 . 1.3908(14) ? N1 C8 . 1.4262(14) ? N3 H3 . 0.8800 ? N3 C2 . 1.3685(15) ? N3 C3A . 1.3872(15) ? C7A C3A . 1.3976(15) ? C7A C7 . 1.3821(16) ? C8 C9 . 1.3910(17) ? C8 C13 . 1.3911(16) ? C3A C4 . 1.3793(16) ? C7 H7 . 0.9500 ? C7 C6 . 1.3933(17) ? C4 H4 . 0.9500 ? C4 C5 . 1.3939(17) ? C5 H5 . 0.9500 ? C5 C6 . 1.3928(17) ? C9 H9 . 0.9500 ? C9 C10 . 1.3880(17) ? C13 H13 . 0.9500 ? C13 C12 . 1.3912(17) ? C6 H6 . 0.9500 ? C12 H12 . 0.9500 ? C12 C11 . 1.383(2) ? C11 H11 . 0.9500 ? C11 C10 . 1.387(2) ? C10 H10 . 0.9500 ? 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 N3 H3 O1 5_656 0.88 2.00 2.8453(13) 174 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 C7A C3A N3 . . . . -0.32(12) ? N1 C7A C3A C4 . . . . 179.08(10) ? N1 C7A C7 C6 . . . . 179.56(11) ? N1 C8 C9 C10 . . . . 177.03(11) ? N1 C8 C13 C12 . . . . -177.13(11) ? N3 C3A C4 C5 . . . . -179.65(11) ? C7A N1 C2 O1 . . . . 178.21(11) ? C7A N1 C2 N3 . . . . -2.59(12) ? C7A N1 C8 C9 . . . . -129.31(12) ? C7A N1 C8 C13 . . . . 48.81(16) ? C7A C3A C4 C5 . . . . 1.11(17) ? C7A C7 C6 C5 . . . . 0.27(17) ? C2 N1 C7A C3A . . . . 1.81(12) ? C2 N1 C7A C7 . . . . -175.82(12) ? C2 N1 C8 C9 . . . . 44.70(17) ? C2 N1 C8 C13 . . . . -137.18(12) ? C2 N3 C3A C7A . . . . -1.31(13) ? C2 N3 C3A C4 . . . . 179.37(12) ? C8 N1 C7A C3A . . . . 176.62(10) ? C8 N1 C7A C7 . . . . -1.01(19) ? C8 N1 C2 O1 . . . . 3.36(19) ? C8 N1 C2 N3 . . . . -177.43(10) ? C8 C9 C10 C11 . . . . 0.53(19) ? C8 C13 C12 C11 . . . . -0.35(19) ? C3A N3 C2 O1 . . . . -178.39(11) ? C3A N3 C2 N1 . . . . 2.40(12) ? C3A C7A C7 C6 . . . . 2.22(16) ? C3A C4 C5 C6 . . . . 1.38(17) ? C7 C7A C3A N3 . . . . 177.61(10) ? C7 C7A C3A C4 . . . . -2.99(17) ? C4 C5 C6 C7 . . . . -2.11(18) ? C9 C8 C13 C12 . . . . 0.98(18) ? C13 C8 C9 C10 . . . . -1.07(18) ? C13 C12 C11 C10 . . . . -0.2(2) ? C12 C11 C10 C9 . . . . 0.1(2) ?