#------------------------------------------------------------------------------ #$Date: 2024-02-03 04:03:35 +0100 (Sat, 03 Feb 2024) $ #$Revision: 289303 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/30/2023023.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_2023023 loop_ _publ_author_name 'Montoya-Garcia, Maribel' 'Cortes-Hernandez, H\'ector' 'D'Vries, Richard' 'Valencia-Sanchez, Hoover' _publ_section_title ; Crystal structure, Hirsfeld surface analysis and DFT study of N-(2-nitrophenyl)maleimide ; _journal_coeditor_code VU2003 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989024000926 _journal_volume 80 _journal_year 2024 _chemical_formula_iupac 'C10 H6 N2 O4' _chemical_formula_moiety 'C10 H6 N2 O4' _chemical_formula_sum 'C10 H6 N2 O4' _chemical_formula_weight 218.17 _chemical_name_common ; N-(2-Nitrophenyl)maleimide ; _chemical_name_systematic ; 1-(2-Nitrophenyl)pyrrole-2,5-dione ; _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 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 91.969(5) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.331(5) _cell_length_b 7.769(5) _cell_length_c 17.558(5) _cell_measurement_reflns_used 2214 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.4914 _cell_measurement_theta_min 3.6101 _cell_volume 1953.7(15) _computing_cell_refinement ; CrysAlisPro (Agilent, 2012) ; _computing_data_collection ; CrysAlisPro (Agilent, 2012) ; _computing_data_reduction ; CrysAlisPro (Agilent, 2012) ; _computing_molecular_graphics ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_publication_material ; Olex2 1.3 (Dolomanov et al., 2009) ; _computing_structure_refinement ; SHELXL2016/6 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014/5 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.877 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8808 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.968 _diffrn_reflns_theta_min 3.610 _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; (CrysAlisPro; Agilent, 2012) ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.5963 _exptl_crystal_size_mid 0.5082 _exptl_crystal_size_min 0.3633 _refine_diff_density_max 0.206 _refine_diff_density_min -0.194 _refine_ls_extinction_coef 0.0083(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method ; SHELXL2016/6 (Sheldrick, 2015b) ; _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 4548 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.020 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0479 _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^)+(0.0388P)^2^+0.6076P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0988 _refine_ls_wR_factor_ref 0.1215 _reflns_number_gt 2815 _reflns_number_total 5183 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file vu2003sup1.cif _cod_data_source_block I _cod_database_code 2023023 _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_hkl_file ; 0 0 4 4665.98 17.16 0 0 5 0.75 0.88 0 0 -6 8434.65 28.06 0 0 6 8396.89 28.47 0 0 7 8.25 1.61 0 0 -7 10.72 1.26 0 0 -8 4.40 0.79 0 0 8 3.66 0.89 0 0 -9 0.62 0.55 0 0 9 0.07 0.65 0 0 10 72.07 3.56 0 0 -10 73.64 3.49 0 0 -11 -0.21 0.67 0 0 11 -0.91 1.04 0 0 12 133.67 5.40 0 0 -12 135.95 5.22 0 0 -13 -0.26 0.60 0 0 13 0.21 0.95 0 0 -14 12.60 1.87 0 0 14 12.08 1.95 0 0 15 -0.12 1.14 0 0 16 26.73 2.90 0 0 17 -1.59 1.31 0 0 18 0.97 1.20 0 0 19 0.14 1.15 0 0 20 1.37 1.36 0 0 21 -0.72 1.20 0 0 22 2.68 1.71 0 0 23 3.66 1.79 0 0 24 1.49 1.46 0 1 3 2556.56 14.12 0 -1 4 2357.73 10.16 0 1 4 2301.03 14.75 0 1 5 78.26 3.09 0 -1 5 77.93 2.14 0 -1 6 1324.50 9.99 0 1 6 1302.57 13.11 0 1 7 6.49 1.41 0 1 -7 4.96 0.80 0 -1 8 559.76 7.84 0 1 8 565.84 9.61 0 1 -8 556.64 7.69 0 -1 -9 92.92 4.04 0 -1 9 93.14 3.48 0 1 9 97.38 4.35 0 1 -9 101.32 3.54 0 1 10 6.31 1.38 0 1 -10 7.96 1.14 0 -1 -10 10.13 1.43 0 -1 11 -0.88 0.80 0 1 11 -1.86 1.32 0 -1 -11 0.62 0.70 0 1 -11 -0.36 0.59 0 -1 12 7.65 1.33 0 1 12 6.25 1.48 0 -1 -12 6.13 1.29 0 1 13 33.75 3.08 0 -1 -13 30.23 2.75 0 -1 13 28.63 2.55 0 -1 14 31.79 2.85 0 1 14 33.74 3.20 0 -1 15 0.63 0.99 0 1 15 1.16 1.05 0 1 16 14.73 2.48 0 -1 16 12.94 2.06 0 -1 17 2.86 1.25 0 1 17 2.00 1.43 0 -1 18 9.71 1.93 0 1 18 6.57 2.00 0 -1 19 2.79 1.38 0 1 19 1.36 1.31 0 -1 20 2.16 1.35 0 1 20 1.58 1.44 0 -1 21 0.53 1.08 0 1 21 -0.11 1.16 0 1 22 6.75 2.02 0 -1 22 5.35 1.81 0 1 23 4.10 2.14 0 1 24 1.41 1.64 0 -2 0 0.98 0.35 0 2 0 0.65 0.34 0 2 1 3411.20 16.40 0 -2 1 3373.83 13.71 0 2 -1 3406.75 13.63 0 2 -2 144.63 2.61 0 -2 2 144.66 2.64 0 2 2 144.23 3.70 0 2 3 81.09 3.04 0 2 -3 86.67 1.91 0 -2 3 85.75 1.97 0 -2 4 567.44 5.18 0 2 4 594.93 8.61 0 -2 5 550.44 5.47 0 2 5 543.58 8.80 0 2 6 331.47 7.26 0 -2 6 318.46 4.47 0 2 7 67.53 3.60 0 -2 7 69.36 2.29 0 2 8 351.36 8.28 0 -2 8 340.94 5.55 0 -2 9 19.72 1.52 0 2 9 17.10 2.05 0 -2 10 123.20 3.96 0 2 10 116.31 5.39 0 2 11 46.76 3.58 0 -2 -11 48.45 3.40 0 -2 11 43.83 2.58 0 -2 12 69.24 3.37 0 2 12 59.89 4.20 0 -2 -12 67.30 4.13 0 -2 13 12.43 1.59 0 2 13 12.60 2.24 0 -2 -13 10.39 0.74 0 -2 14 1.41 0.25 0 -2 14 2.29 1.05 0 2 14 2.26 1.18 0 -2 15 24.18 2.41 0 2 15 29.02 3.25 0 -2 16 8.09 1.61 0 2 16 5.31 1.65 0 -2 17 0.89 0.87 0 2 17 1.53 1.14 0 2 18 1.82 1.29 0 -2 18 2.72 1.21 0 2 19 1.92 1.39 0 -2 19 3.23 1.31 0 -2 20 3.33 1.30 0 2 20 7.57 2.32 0 2 21 -0.20 1.29 0 2 22 1.40 1.62 0 -3 0 0.66 0.44 0 3 0 0.05 0.53 0 3 -1 96.77 2.96 0 -3 1 98.55 2.96 0 3 1 95.86 3.38 0 -3 -1 98.64 3.34 0 3 2 15.75 1.51 0 3 -2 14.05 1.12 0 -3 2 12.50 1.01 0 -3 -2 12.96 1.33 0 3 -3 56.92 1.99 0 -3 3 53.60 1.97 0 3 3 54.75 2.84 0 3 4 60.03 3.17 0 -3 4 55.83 1.97 0 3 -4 58.20 1.92 0 -3 5 1826.29 11.10 0 3 5 1894.15 18.19 0 3 6 177.45 6.02 0 -3 6 183.13 3.62 0 -3 7 11.72 0.97 0 -3 7 13.00 1.06 0 3 7 11.73 1.83 0 -3 8 575.78 7.06 0 -3 8 557.86 6.67 0 3 8 557.70 11.34 0 -3 9 89.17 2.90 0 3 9 87.78 4.84 0 -3 9 86.80 2.91 0 3 10 6.38 1.56 0 -3 10 7.43 0.99 0 -3 10 8.57 1.10 0 -3 -10 6.96 1.45 0 3 11 51.69 4.07 0 -3 11 59.87 2.77 0 -3 12 0.33 0.63 0 3 12 0.54 1.15 0 -3 13 140.49 4.68 0 3 13 139.71 6.86 0 3 14 0.51 1.06 0 -3 14 1.16 0.73 0 3 15 -1.08 1.70 0 -3 15 1.35 0.85 0 -3 16 8.47 1.53 0 3 16 8.13 2.24 0 -3 17 -0.93 0.98 0 3 17 -0.33 1.33 0 -3 18 -1.27 0.99 0 3 18 0.30 1.20 0 3 19 -0.17 1.47 0 3 20 3.86 1.77 0 3 21 6.97 2.13 0 4 0 663.94 9.62 0 -4 0 681.98 9.52 0 4 1 264.60 6.37 0 4 -1 268.07 5.81 0 -4 -1 274.12 6.38 0 -4 1 267.81 5.75 0 -4 2 6.38 0.91 0 4 2 4.02 0.90 0 4 -2 6.21 0.90 0 -4 -2 5.06 1.03 0 -4 3 5.78 0.81 0 4 -3 5.69 0.84 0 4 3 7.00 1.16 0 -4 -3 6.00 1.09 0 4 4 -0.44 0.89 0 -4 -4 -0.23 0.58 0 -4 4 0.11 0.38 0 4 -4 0.08 0.42 0 4 -5 9.67 0.96 0 4 5 8.72 1.51 0 -4 5 8.80 0.91 0 -4 -5 5.30 1.11 0 -4 -6 240.99 7.27 0 4 6 234.29 7.43 0 -4 6 225.21 4.41 0 -4 -7 2.97 0.94 0 -4 7 3.27 0.59 0 -4 -8 3.74 1.11 0 4 8 3.31 1.29 0 -4 8 4.51 0.68 0 -4 9 19.34 1.37 0 -4 9 19.21 1.31 0 4 9 19.47 2.54 0 -4 10 87.37 2.88 0 -4 10 86.67 2.99 0 4 10 91.24 5.43 0 -4 11 3.19 0.74 0 -4 11 3.40 0.72 0 4 11 2.10 1.49 0 4 12 -0.32 1.33 0 -4 12 0.00 0.50 0 -4 12 1.36 0.74 0 -4 13 23.60 1.81 0 -4 13 25.09 1.90 0 4 13 22.38 3.14 0 4 14 32.90 3.92 0 -4 14 38.96 2.40 0 -4 14 36.08 2.34 0 4 15 0.37 1.36 0 -4 15 -0.01 0.62 0 4 16 24.48 3.70 0 -4 16 23.79 2.09 0 4 17 0.36 1.34 0 4 18 2.63 1.83 0 4 19 -3.43 1.77 0 4 20 -0.64 1.44 0 -5 0 -0.60 0.60 0 5 0 -0.91 0.77 0 5 1 11.58 1.59 0 -5 1 11.18 1.39 0 -5 -1 12.92 1.61 0 5 -1 10.83 1.44 0 -5 -2 134.49 5.17 0 5 -2 144.61 4.65 0 5 2 140.63 5.35 0 -5 2 140.63 4.51 0 -5 3 20.29 1.69 0 5 -3 22.28 1.77 0 5 3 19.13 2.15 0 -5 -3 20.40 2.16 0 -5 -4 22.16 2.29 0 5 -4 22.29 1.68 0 5 4 19.28 2.25 0 -5 4 19.59 1.60 0 -5 -5 15.55 1.99 0 5 5 15.05 2.25 0 -5 5 14.64 1.35 0 5 -5 16.80 1.40 0 -5 6 133.38 3.78 0 -5 -6 137.60 5.94 0 5 6 141.52 6.29 0 5 7 57.08 4.21 0 -5 7 63.08 2.52 0 -5 8 94.91 3.02 0 5 8 100.23 5.66 0 -5 9 53.28 2.15 0 -5 9 52.77 2.26 0 5 9 48.19 4.15 0 -5 10 34.90 1.74 0 -5 10 34.41 1.82 0 5 10 37.52 3.81 0 5 11 7.22 2.03 0 -5 11 5.63 0.80 0 -5 11 6.22 0.84 0 -5 12 0.53 0.44 0 5 12 -1.42 1.73 0 -5 12 -0.12 0.39 0 -5 13 -0.36 0.43 0 5 13 0.65 1.31 0 -5 14 10.47 1.16 0 5 14 13.02 2.68 0 5 15 1.30 1.40 0 5 16 0.13 1.38 0 5 17 1.45 1.43 0 5 18 -0.61 1.72 0 -6 0 679.34 11.78 0 6 0 673.21 11.94 0 6 -1 15.94 2.09 0 6 1 13.18 2.07 0 -6 -1 15.79 1.96 0 -6 1 12.77 1.75 0 6 -2 166.49 5.56 0 6 2 163.11 6.41 0 -6 -2 175.88 6.41 0 -6 2 170.24 5.57 0 6 -3 1.64 0.78 0 6 3 0.95 1.17 0 -6 3 0.77 0.68 0 -6 -3 0.19 0.70 0 -6 4 42.48 2.58 0 -6 -4 41.43 3.42 0 6 4 50.68 3.83 0 6 -4 48.19 2.75 0 6 5 2.40 1.39 0 6 -5 1.54 0.76 0 -6 5 0.63 0.59 0 6 -6 157.01 4.34 0 -6 6 146.80 4.41 0 6 6 148.65 6.93 0 -6 7 105.72 3.55 0 6 7 107.77 6.08 0 -6 8 0.57 0.37 0 6 8 3.59 1.80 0 6 9 10.47 2.37 0 -6 9 9.19 0.99 0 -6 10 0.49 0.36 0 6 10 0.83 1.23 0 -6 10 0.72 0.36 0 6 11 -4.49 1.80 0 -6 11 0.34 0.31 0 6 12 -0.23 1.17 0 6 13 1.69 1.61 0 6 14 9.31 2.63 0 6 15 0.96 1.38 0 6 16 5.34 2.06 0 6 17 3.25 1.86 0 7 0 -1.32 1.16 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2.32 1.16 1 0 14 0.47 0.90 -1 0 -14 0.46 0.58 -1 0 -15 0.80 0.90 1 0 15 3.16 1.25 1 0 16 -0.11 0.93 1 0 17 8.62 1.84 1 0 18 -1.43 1.39 1 0 19 21.31 3.01 1 0 20 1.58 1.23 1 0 21 6.78 1.97 1 0 22 1.66 1.44 1 0 23 1.82 1.40 -1 1 23 -0.56 1.22 -1 1 22 2.44 1.73 -1 -1 22 1.73 1.33 -1 1 21 -1.00 1.40 -1 -1 21 0.73 1.20 -1 -1 20 2.91 1.40 -1 1 20 4.33 1.68 -1 -1 19 2.17 1.31 -1 1 19 0.74 1.18 -1 -1 18 16.92 2.44 -1 1 18 12.86 2.47 -1 -1 17 -0.45 1.14 -1 1 17 -1.44 1.53 -1 -1 16 14.81 2.15 -1 1 16 18.56 2.76 -1 1 15 0.68 1.07 -1 -1 15 1.09 0.92 -1 1 14 6.83 1.68 -1 -1 14 6.46 1.47 -1 1 13 0.31 0.90 1 -1 -13 4.55 1.27 -1 -1 13 2.28 1.42 1 -1 -12 414.97 9.76 -1 1 12 408.06 9.90 -1 -1 12 405.61 8.74 -1 -1 11 157.57 5.23 1 -1 -11 168.57 5.94 -1 1 11 154.97 5.91 1 -1 -10 34.57 2.62 1 -1 -10 33.04 0.99 -1 -1 10 36.09 2.41 -1 1 10 38.37 2.87 -1 -1 9 7.37 1.08 -1 1 9 6.01 1.22 1 -1 -9 6.45 0.53 -1 -1 8 129.81 3.92 -1 1 8 119.57 4.46 1 -1 -8 119.74 2.30 -1 1 7 20.07 1.98 -1 -1 7 19.18 1.48 -1 1 6 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15 4 5 21.65 3.63 -15 -4 -6 0.75 1.36 15 4 6 3.44 1.77 -15 -4 -7 2.02 1.55 15 4 7 5.50 2.19 -15 -4 -8 0.62 1.09 15 4 8 0.24 1.28 -15 -4 -9 -0.10 1.08 -15 -4 -10 -0.52 1.25 -15 -4 -11 -0.03 1.20 -15 -4 -12 4.42 1.77 -15 5 9 1.58 1.69 -15 5 8 0.93 1.47 -15 5 7 1.85 1.56 -15 5 6 7.96 2.08 -15 5 5 2.22 1.30 -15 5 4 -0.01 1.21 -15 5 3 -1.55 1.18 -15 5 2 3.76 1.45 15 5 -1 -1.69 1.57 15 5 0 6.07 2.38 15 5 1 0.87 1.57 15 5 2 5.48 2.15 15 5 3 10.11 2.84 -15 -5 -7 9.53 2.70 -15 6 8 -2.06 1.40 -15 6 7 0.21 1.21 -15 6 6 -2.10 1.51 -16 0 11 -0.55 1.20 -16 0 10 14.84 3.06 -16 0 10 14.42 2.83 -16 0 9 0.27 1.40 -16 0 8 1.56 1.24 -16 0 7 -1.61 1.61 -16 0 6 0.53 1.32 -16 0 5 0.43 1.28 -16 0 4 -2.47 1.64 -16 0 3 3.12 2.03 -16 0 2 1.46 1.25 -16 0 1 -0.13 1.15 -16 0 0 8.11 2.16 -16 0 -1 1.50 1.68 -16 0 -2 5.91 2.17 -16 0 -3 3.08 1.42 -16 0 -4 2.98 1.67 -16 0 -5 -1.88 1.55 -16 0 -6 6.65 1.98 -16 0 -7 1.76 1.46 -16 0 -8 2.41 1.33 16 0 9 1.56 1.36 -16 0 -9 0.92 1.36 16 0 10 1.07 1.25 16 0 11 -1.35 1.66 -16 -1 14 0.23 1.41 -16 -1 13 -1.33 1.45 -16 -1 12 6.55 2.02 -16 -1 11 2.31 1.55 -16 1 10 2.75 1.51 -16 -1 10 4.16 1.80 -16 1 9 0.84 1.68 -16 -1 9 1.62 1.47 -16 1 8 1.79 1.37 -16 -1 8 -0.79 1.71 -16 -1 7 9.74 2.30 -16 -1 6 2.33 1.24 -16 -1 5 -0.38 1.34 -16 -1 4 9.72 2.24 -16 -1 3 1.27 1.53 -16 1 2 1.19 1.47 -16 -1 2 -0.38 1.51 -16 1 1 17.94 2.98 -16 -1 1 13.82 2.82 -16 1 0 19.41 3.15 -16 -1 0 14.40 2.67 -16 -1 -1 4.17 1.84 -16 -1 -2 0.81 1.15 -16 -1 -3 3.23 1.75 -16 -1 -4 -0.34 1.38 -16 -1 -5 5.18 1.71 16 1 6 -0.01 1.32 -16 -1 -6 -0.34 1.42 16 1 7 1.10 1.19 -16 -1 -7 -2.88 1.81 16 1 8 1.73 1.59 -16 -1 -8 3.36 1.54 16 1 9 1.28 1.25 -16 -1 -9 -1.81 1.52 16 1 10 1.21 1.53 -16 -1 -10 -2.58 1.62 16 1 11 -0.14 1.38 -16 -1 -11 -0.74 1.11 16 1 12 0.79 1.37 -16 -1 -12 -0.36 1.19 -16 -2 14 7.64 2.32 -16 -2 13 2.00 1.64 -16 -2 12 1.86 1.31 -16 -2 11 4.66 1.78 -16 2 10 0.54 1.16 -16 -2 10 0.45 1.46 -16 2 9 6.88 2.32 -16 -2 9 4.82 1.92 -16 2 8 3.09 1.94 -16 -2 8 3.29 1.50 -16 -2 7 4.54 1.90 -16 2 7 4.26 1.79 -16 -2 6 2.00 1.54 -16 2 6 -0.64 1.70 -16 -2 5 -1.51 1.50 -16 2 5 -0.82 1.51 -16 -2 4 0.05 1.36 -16 -2 3 0.46 1.11 -16 -2 2 4.57 1.82 -16 -2 1 6.19 2.07 -16 -2 0 2.33 1.49 -16 -2 -1 5.05 1.94 -16 -2 -2 1.30 1.83 -16 -2 -3 3.68 1.91 -16 -2 -4 1.24 1.41 16 2 4 -0.37 1.23 -16 -2 -5 0.62 1.23 16 2 5 -1.52 1.51 16 2 6 0.88 1.22 -16 -2 -6 2.62 1.73 16 2 7 3.57 1.61 -16 -2 -7 1.22 1.50 16 2 8 0.97 1.19 -16 -2 -8 1.66 1.45 16 2 9 13.39 2.83 -16 -2 -9 9.79 2.37 16 2 10 2.45 1.77 -16 -2 -10 -0.08 1.48 16 2 11 0.19 1.34 -16 -2 -11 1.99 1.03 16 2 12 0.72 1.59 -16 -2 -12 -2.81 1.53 -16 -3 13 -1.39 1.74 -16 -3 12 -0.39 1.31 -16 -3 11 2.81 1.62 -16 -3 10 0.54 1.35 -16 -3 9 -2.47 1.85 -16 3 9 5.22 2.06 -16 -3 8 2.71 1.63 -16 3 8 -1.04 1.46 -16 -3 7 11.99 2.75 -16 3 7 10.28 2.33 -16 -3 6 1.67 1.59 -16 3 6 1.50 1.58 -16 -3 5 6.62 2.21 -16 3 5 8.87 2.25 -16 -3 4 5.49 1.87 -16 3 4 6.11 1.96 -16 -3 3 7.79 2.33 -16 3 3 7.71 2.01 -16 -3 2 14.91 3.07 -16 3 2 10.37 2.15 -16 -3 1 8.22 2.44 -16 3 1 6.61 1.89 -16 -3 0 10.02 2.63 -16 3 0 10.11 2.12 -16 -3 -1 16.57 3.17 -16 -3 -2 1.39 1.72 16 3 2 2.97 1.60 -16 -3 -3 2.40 1.84 16 3 3 3.29 1.57 -16 -3 -4 4.86 2.00 16 3 4 5.92 1.78 -16 -3 -5 3.14 1.71 16 3 5 2.44 1.69 -16 -3 -6 0.22 1.33 16 3 6 4.43 1.81 -16 -3 -7 1.00 1.50 16 3 7 2.53 1.77 -16 -3 -8 -0.32 1.27 16 3 8 -0.43 1.14 -16 -3 -9 6.48 2.15 16 3 9 0.94 1.46 -16 -3 -10 -0.68 1.21 -16 -3 -11 -3.92 1.74 -16 4 9 -0.01 1.34 -16 4 8 1.83 1.48 -16 -4 7 0.12 1.28 -16 4 7 2.13 1.70 -16 -4 6 -3.19 1.80 -16 4 6 -0.46 1.29 -16 -4 5 7.53 2.25 -16 4 5 4.54 1.81 -16 4 4 0.01 1.10 -16 -4 4 7.37 2.36 -16 -4 3 5.51 1.97 -16 4 3 1.54 1.12 -16 -4 2 1.24 1.25 -16 4 2 2.54 1.42 -16 -4 1 6.53 2.37 -16 4 1 2.22 1.19 -16 -4 0 -2.52 1.76 -16 4 0 2.95 1.40 -16 -4 -1 0.70 1.21 16 4 1 0.73 1.28 -16 -4 -2 5.54 2.10 16 4 2 5.96 2.06 -16 -4 -3 2.87 1.96 16 4 3 0.38 1.55 -16 -4 -4 7.22 2.35 16 4 4 3.75 1.74 -16 -4 -5 3.77 1.55 -16 -4 -6 4.33 2.04 -16 -4 -7 2.09 1.58 -16 5 8 1.21 1.33 -16 5 7 0.50 1.60 -16 5 6 2.78 1.49 -16 5 5 -2.07 1.32 -16 5 4 -3.21 1.56 -17 0 10 1.49 1.47 -17 0 9 1.10 1.29 -17 0 8 -0.96 1.43 -17 0 7 4.61 1.80 -17 0 6 -1.59 1.20 -17 0 5 -0.83 1.34 -17 0 4 0.10 1.14 -17 0 3 10.72 2.58 -17 0 2 1.02 1.30 -17 0 1 -1.57 1.61 -17 0 0 0.42 1.45 -17 0 -1 -0.27 1.53 -17 0 -2 -0.94 1.10 -17 0 -3 1.03 1.42 -17 0 -4 1.97 1.54 -17 0 -5 0.45 1.27 -17 0 -6 -3.59 1.84 -17 0 -7 3.52 1.93 -17 0 -8 0.26 1.21 -17 -1 11 0.89 1.24 -17 -1 10 2.15 1.84 -17 -1 9 11.69 2.74 -17 1 8 6.63 2.41 -17 -1 8 5.86 2.16 -17 1 7 7.55 2.22 -17 -1 7 7.00 2.06 -17 -1 6 -1.24 1.50 -17 -1 5 -2.37 1.94 -17 -1 4 0.75 1.10 -17 -1 3 0.36 1.25 -17 -1 2 -0.98 1.43 -17 -1 1 2.03 1.56 -17 -1 0 0.49 1.39 -17 -1 -1 16.86 3.09 -17 -1 -2 2.26 1.43 -17 -1 -3 -2.71 1.96 -17 -1 -4 4.93 1.73 -17 -1 -5 -1.43 1.69 -17 -1 -6 -0.24 1.38 -17 -1 -7 1.05 1.31 17 1 8 2.94 1.43 -17 -1 -8 1.78 1.47 17 1 9 -0.92 1.34 -17 -1 -9 -0.76 1.29 17 1 10 -1.85 1.57 -17 -1 -10 3.13 1.62 17 1 11 -4.08 1.81 -17 -1 -11 -0.43 1.28 -17 -2 9 1.96 1.46 -17 2 8 2.69 1.68 -17 -2 8 -1.91 1.49 -17 2 7 -3.12 1.89 -17 -2 7 0.43 1.20 -17 2 6 -0.69 1.08 -17 -2 6 2.53 1.81 -17 2 5 0.10 1.47 -17 -2 5 0.96 1.21 -17 2 4 0.82 1.25 -17 -2 4 3.53 1.77 -17 -2 3 12.51 2.88 -17 -2 2 6.92 2.24 -17 -2 1 1.06 1.32 -17 -2 0 0.68 1.47 -17 -2 -1 -1.87 1.41 -17 -2 -2 4.11 2.02 -17 -2 -3 3.20 1.74 -17 -2 -4 1.26 1.43 17 2 5 0.54 1.43 -17 -2 -5 -1.26 1.28 17 2 6 1.15 1.29 -17 -2 -6 3.82 1.76 17 2 7 -8.01 2.27 -17 -2 -7 4.08 2.01 17 2 8 0.56 1.34 -17 -2 -8 -0.16 1.48 17 2 9 11.88 2.91 -17 3 7 0.76 1.64 -17 3 6 1.24 1.54 -17 3 5 4.65 1.98 -17 -3 4 1.55 1.34 -17 3 4 0.50 1.26 -17 -3 3 -0.22 1.20 -17 3 3 2.34 1.31 -17 -3 2 1.30 1.25 -17 3 2 -1.96 1.65 -17 -3 1 2.41 1.52 -17 3 1 1.42 1.27 -17 -3 0 0.70 1.22 -17 3 0 1.25 1.13 -17 -3 -1 0.50 1.31 -17 3 -1 -0.10 1.28 -17 -3 -2 5.08 2.19 -17 -3 -3 -0.88 1.35 17 3 3 -0.06 1.51 17 3 4 1.47 1.60 -17 4 7 8.70 2.37 -17 4 6 -0.56 1.28 -17 4 5 11.57 2.57 -17 4 4 1.46 1.38 -17 4 3 4.76 1.68 -17 4 2 1.52 1.32 -18 2 5 0.03 1.21 -18 2 4 -2.37 1.65 -18 3 5 2.30 1.62 -18 3 4 0.98 1.86 -18 3 3 9.20 2.11 -18 3 2 -1.83 1.66 -18 3 1 0.12 1.07 -18 3 0 1.80 1.18 -18 4 5 2.09 1.44 -18 4 4 5.51 2.20 0 0 0 0.00 0.00 TITL yoeA-c in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 14.331252 7.769125 17.557839 90.0000 91.9689 90.0000 ZERR 8.00 0.001251 0.000627 0.001390 0.0000 0.0072 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 88.00 80.00 8.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_res_file ; TITL shelx_a.res in P2(1)/n shelx.res created by SHELXL-2016/6 at 11:34:30 on 11-Oct-2023 REM Old TITL REM SHELXT solution in P2(1)/n REM R1 0.193, Rweak 0.011, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C23 N3 O6 CELL 0.71073 14.331 7.769 17.558 90 91.969 90 ZERR 8 0.005 0.005 0.005 0 0.005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 80 48 16 32 L.S. 10 PLAN 16 TEMP 20(2) CONF BOND $H list 4 MORE -1 fmap 2 ACTA OMIT -5 58 REM REM REM WGHT 0.038800 0.607600 EXTI 0.008262 FVAR 0.53191 N2 3 0.577409 0.704790 0.175029 11.00000 0.03709 0.04948 = 0.04744 -0.01114 -0.00324 0.00308 O6 4 0.470028 0.643008 0.078156 11.00000 0.05864 0.09799 = 0.05817 -0.02295 -0.01342 0.00625 O8 4 0.428329 0.532966 0.238700 11.00000 0.08528 0.03760 = 0.09587 0.00381 0.01600 -0.00445 N1 3 0.237198 0.496672 0.462837 11.00000 0.03985 0.05369 = 0.04945 0.01062 0.00299 0.00472 O5 4 0.704418 0.676717 0.258074 11.00000 0.05925 0.10781 = 0.07390 -0.02660 -0.02237 0.02785 N4 3 0.387023 0.666619 0.225012 11.00000 0.04866 0.05084 = 0.05690 0.00131 0.00344 -0.01183 O2 4 0.111549 0.428852 0.534952 11.00000 0.05671 0.09736 = 0.09246 0.03357 0.02000 -0.00012 O7 4 0.304252 0.674810 0.206300 11.00000 0.04745 0.09682 = 0.09727 -0.00056 -0.00770 -0.02759 O1 4 0.334307 0.656767 0.389298 11.00000 0.05750 0.12587 = 0.09868 0.06147 0.02155 0.00743 C13 1 0.438161 0.828609 0.232767 11.00000 0.03856 0.03542 = 0.04248 0.00413 -0.00254 -0.00174 C14 1 0.530099 0.842086 0.210446 11.00000 0.03633 0.04163 = 0.04053 -0.00252 -0.00272 -0.00024 N3 3 0.377266 0.606217 0.574132 11.00000 0.07689 0.08197 = 0.05838 -0.01542 -0.01124 -0.00047 PART 1 O4A 4 0.301503 0.680589 0.588007 10.50000 0.13513 0.13340 = 0.11875 -0.04160 0.02459 0.03560 PART 0 C4 1 0.302109 0.378506 0.495814 11.00000 0.04356 0.04911 = 0.04512 0.00690 0.00651 0.00544 C12 1 0.392608 0.965896 0.264340 11.00000 0.04417 0.04735 = 0.05659 0.00663 0.00581 0.00748 AFIX 43 H12 2 0.330597 0.955447 0.277613 11.00000 -1.20000 AFIX 0 C15 1 0.575530 0.997577 0.221271 11.00000 0.04510 0.05429 = 0.05223 -0.00387 0.00259 -0.01208 AFIX 43 H15 2 0.636591 1.010733 0.205935 11.00000 -1.20000 AFIX 0 C20 1 0.543333 0.614323 0.111384 11.00000 0.04976 0.05682 = 0.04756 -0.00891 0.00184 -0.00550 C17 1 0.661026 0.631883 0.201827 11.00000 0.04334 0.06236 = 0.05330 -0.00565 -0.00127 0.00831 C3 1 0.370543 0.426755 0.548876 11.00000 0.05325 0.06102 = 0.04278 0.00030 0.00223 0.01002 C7 1 0.146237 0.515510 0.486409 11.00000 0.04214 0.06198 = 0.05745 0.00734 0.00457 -0.00050 C11 1 0.439251 1.117845 0.276048 11.00000 0.07088 0.04067 = 0.06094 -0.00095 0.00899 0.00934 AFIX 43 H11 2 0.409483 1.210544 0.298310 11.00000 -1.20000 AFIX 0 C16 1 0.530493 1.132831 0.254703 11.00000 0.07533 0.04231 = 0.06175 -0.00746 0.00351 -0.01587 AFIX 43 H16 2 0.562129 1.236008 0.263028 11.00000 -1.20000 AFIX 0 C10 1 0.258289 0.629135 0.413211 11.00000 0.05150 0.07016 = 0.05202 0.01763 0.00236 0.00168 O3 4 0.455937 0.666132 0.585587 11.00000 0.10284 0.13165 = 0.11927 -0.03967 -0.01802 -0.02742 C19 1 0.613684 0.481199 0.096085 11.00000 0.06496 0.05756 = 0.06090 -0.01905 0.01053 -0.00048 AFIX 43 H19 2 0.610624 0.403119 0.055928 11.00000 -1.20000 AFIX 0 C9 1 0.170667 0.725942 0.400282 11.00000 0.06059 0.06748 = 0.06693 0.02226 -0.00748 0.00838 AFIX 43 H9 2 0.162690 0.819245 0.367519 11.00000 -1.20000 AFIX 0 C5 1 0.298369 0.207693 0.474168 11.00000 0.06898 0.05473 = 0.06814 0.00293 0.00151 -0.00036 AFIX 43 H5 2 0.253871 0.171906 0.437746 11.00000 -1.20000 AFIX 0 C18 1 0.681042 0.490684 0.148093 11.00000 0.06012 0.06299 = 0.06903 -0.00830 0.00959 0.01634 AFIX 43 H18 2 0.733352 0.419827 0.150902 11.00000 -1.20000 AFIX 0 C8 1 0.106130 0.660140 0.442016 11.00000 0.04742 0.07467 = 0.07347 0.01086 0.00073 0.01557 AFIX 43 H8 2 0.044719 0.698340 0.443510 11.00000 -1.20000 AFIX 0 C2 1 0.433818 0.310661 0.579696 11.00000 0.06145 0.10038 = 0.05400 0.01124 -0.00127 0.02351 AFIX 43 H2 2 0.480623 0.346376 0.614146 11.00000 -1.20000 AFIX 0 C1 1 0.426335 0.141091 0.558486 11.00000 0.07966 0.08601 = 0.07664 0.02759 0.01472 0.03926 AFIX 43 H1 2 0.467045 0.060191 0.580155 11.00000 -1.20000 AFIX 0 C6 1 0.359789 0.090240 0.505963 11.00000 0.09485 0.05140 = 0.09537 0.00941 0.01682 0.01687 AFIX 43 H6 2 0.355932 -0.024794 0.491543 11.00000 -1.20000 AFIX 0 PART 2 O4B 4 0.310857 0.691408 0.578421 10.50000 0.08075 0.04007 = 0.10601 -0.01431 -0.02081 0.01526 HKLF 4 REM shelx_a.res in P2(1)/n REM R1 = 0.0479 for 2815 Fo > 4sig(Fo) and 0.0873 for all 4548 data REM 299 parameters refined using 0 restraints END WGHT 0.0388 0.6075 REM Highest difference peak 0.206, deepest hole -0.194, 1-sigma level 0.035 Q1 1 0.4237 0.5749 0.6396 11.00000 0.05 0.21 Q2 1 0.3686 0.5662 0.6647 11.00000 0.05 0.17 Q3 1 0.6616 0.5591 0.2621 11.00000 0.05 0.15 Q4 1 0.1295 0.5456 0.5472 11.00000 0.05 0.14 Q5 1 0.1034 0.4062 0.4826 11.00000 0.05 0.14 Q6 1 0.2462 0.5140 0.4251 11.00000 0.05 0.14 Q7 1 0.4960 0.8271 0.2451 11.00000 0.05 0.14 Q8 1 0.4756 0.8297 0.2180 11.00000 0.05 0.13 Q9 1 0.1579 0.7681 0.4498 11.00000 0.05 0.13 Q10 1 0.6249 0.4309 0.1420 11.00000 0.05 0.13 Q11 1 0.5628 1.0601 0.2663 11.00000 0.05 0.13 Q12 1 0.1394 0.6861 0.3945 11.00000 0.05 0.12 Q13 1 0.5633 0.8863 0.2407 11.00000 0.05 0.12 Q14 1 0.7304 0.5284 0.2540 11.00000 0.05 0.12 Q15 1 0.3353 0.5395 0.3757 11.00000 0.05 0.12 Q16 1 0.7040 0.8136 0.2185 11.00000 0.05 0.12 ; _shelx_res_checksum 64526 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 N N2 0.57741(10) 0.7048(2) 0.17503(8) 0.0448(4) Uani d 1 . . O O6 0.47003(10) 0.6430(2) 0.07816(8) 0.0720(5) Uani d 1 . . O O8 0.42833(12) 0.53297(19) 0.23870(10) 0.0726(5) Uani d 1 . . N N1 0.23720(10) 0.4967(2) 0.46284(9) 0.0476(4) Uani d 1 . . O O5 0.70442(11) 0.6767(2) 0.25807(9) 0.0809(5) Uani d 1 . . N N4 0.38702(12) 0.6666(2) 0.22501(9) 0.0521(4) Uani d 1 . . O O2 0.11155(11) 0.4289(2) 0.53495(10) 0.0818(5) Uani d 1 . . O O7 0.30425(11) 0.6748(2) 0.20630(10) 0.0807(5) Uani d 1 . . O O1 0.33431(11) 0.6568(3) 0.38930(11) 0.0936(6) Uani d 1 . . C C13 0.43816(12) 0.8286(2) 0.23277(10) 0.0389(4) Uani d 1 . . C C14 0.53010(12) 0.8421(2) 0.21045(10) 0.0396(4) Uani d 1 . . N N3 0.37727(17) 0.6062(3) 0.57413(12) 0.0727(6) Uani d 1 . . O O4A 0.3015(11) 0.6806(17) 0.5880(10) 0.129(5) Uani d 0.5 A 1 C C4 0.30211(13) 0.3785(3) 0.49581(10) 0.0458(5) Uani d 1 . . C C12 0.39261(14) 0.9659(2) 0.26434(11) 0.0493(5) Uani d 1 . . H H12 0.330597 0.955447 0.277613 0.059 Uiso calc 1 . . C C15 0.57553(14) 0.9976(3) 0.22127(11) 0.0505(5) Uani d 1 . . H H15 0.636591 1.010733 0.205935 0.061 Uiso calc 1 . . C C20 0.54333(14) 0.6143(3) 0.11138(11) 0.0514(5) Uani d 1 . . C C17 0.66103(13) 0.6319(3) 0.20183(12) 0.0531(5) Uani d 1 . . C C3 0.37054(14) 0.4268(3) 0.54888(11) 0.0523(5) Uani d 1 . . C C7 0.14624(14) 0.5155(3) 0.48641(12) 0.0538(5) Uani d 1 . . C C11 0.43925(16) 1.1178(3) 0.27605(12) 0.0573(5) Uani d 1 . . H H11 0.409483 1.210544 0.298310 0.069 Uiso calc 1 . . C C16 0.53049(16) 1.1328(3) 0.25470(12) 0.0598(6) Uani d 1 . . H H16 0.562129 1.236008 0.263028 0.072 Uiso calc 1 . . C C10 0.25829(15) 0.6291(3) 0.41321(12) 0.0579(6) Uani d 1 . . O O3 0.45594(16) 0.6661(3) 0.58559(13) 0.1184(8) Uani d 1 . . C C19 0.61368(15) 0.4812(3) 0.09608(13) 0.0609(6) Uani d 1 . . H H19 0.610624 0.403119 0.055928 0.073 Uiso calc 1 . . C C9 0.17067(16) 0.7259(3) 0.40028(13) 0.0652(6) Uani d 1 . . H H9 0.162690 0.819245 0.367519 0.078 Uiso calc 1 . . C C5 0.29837(16) 0.2077(3) 0.47417(13) 0.0640(6) Uani d 1 . . H H5 0.253871 0.171906 0.437746 0.077 Uiso calc 1 . . C C18 0.68104(16) 0.4907(3) 0.14809(13) 0.0639(6) Uani d 1 . . H H18 0.733352 0.419827 0.150902 0.077 Uiso calc 1 . . C C8 0.10613(15) 0.6601(3) 0.44202(13) 0.0652(6) Uani d 1 . . H H8 0.044719 0.698340 0.443510 0.078 Uiso calc 1 . . C C2 0.43382(16) 0.3107(4) 0.57970(13) 0.0720(7) Uani d 1 . . H H2 0.480623 0.346376 0.614146 0.086 Uiso calc 1 . . C C1 0.42634(19) 0.1411(4) 0.55849(16) 0.0805(8) Uani d 1 . . H H1 0.467045 0.060191 0.580155 0.097 Uiso calc 1 . . C C6 0.3598(2) 0.0902(3) 0.50596(16) 0.0802(8) Uani d 1 . . H H6 0.355932 -0.024794 0.491543 0.096 Uiso calc 1 . . O O4B 0.3109(8) 0.6914(10) 0.5784(7) 0.076(2) Uani d 0.5 A 2 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 N2 0.0371(8) 0.0495(9) 0.0474(9) 0.0031(7) -0.0032(6) -0.0111(8) O6 0.0586(9) 0.0980(13) 0.0582(9) 0.0062(9) -0.0134(7) -0.0229(9) O8 0.0853(12) 0.0376(8) 0.0959(12) -0.0044(8) 0.0160(9) 0.0038(8) N1 0.0399(9) 0.0537(10) 0.0494(9) 0.0047(7) 0.0030(7) 0.0106(8) O5 0.0592(9) 0.1078(14) 0.0739(10) 0.0278(9) -0.0224(8) -0.0266(10) N4 0.0487(10) 0.0508(11) 0.0569(10) -0.0118(8) 0.0034(8) 0.0013(8) O2 0.0567(10) 0.0974(13) 0.0925(12) -0.0001(9) 0.0200(8) 0.0336(11) O7 0.0474(9) 0.0968(13) 0.0973(12) -0.0276(9) -0.0077(8) -0.0006(10) O1 0.0575(10) 0.1259(16) 0.0987(13) 0.0074(10) 0.0215(9) 0.0615(12) C13 0.0386(9) 0.0354(9) 0.0425(9) -0.0017(8) -0.0025(7) 0.0041(8) C14 0.0363(9) 0.0416(10) 0.0405(9) -0.0002(8) -0.0027(7) -0.0025(8) N3 0.0769(15) 0.0820(16) 0.0584(12) -0.0005(14) -0.0112(11) -0.0154(11) O4A 0.135(9) 0.133(9) 0.119(7) 0.036(6) 0.025(5) -0.042(6) C4 0.0436(10) 0.0491(11) 0.0451(10) 0.0054(9) 0.0065(8) 0.0069(9) C12 0.0442(11) 0.0474(11) 0.0566(12) 0.0075(9) 0.0058(9) 0.0066(10) C15 0.0451(11) 0.0543(12) 0.0522(11) -0.0121(10) 0.0026(8) -0.0039(10) C20 0.0498(11) 0.0568(12) 0.0476(11) -0.0055(10) 0.0018(9) -0.0089(10) C17 0.0433(11) 0.0624(13) 0.0533(12) 0.0083(10) -0.0013(9) -0.0057(10) C3 0.0533(12) 0.0610(13) 0.0428(10) 0.0100(10) 0.0022(9) 0.0003(10) C7 0.0421(11) 0.0620(13) 0.0575(12) -0.0005(10) 0.0046(9) 0.0073(11) C11 0.0709(14) 0.0407(11) 0.0609(13) 0.0093(11) 0.0090(11) -0.0009(10) C16 0.0753(15) 0.0423(11) 0.0618(13) -0.0159(11) 0.0035(11) -0.0075(10) C10 0.0515(12) 0.0702(14) 0.0520(12) 0.0017(11) 0.0024(9) 0.0176(11) O3 0.1028(16) 0.1317(19) 0.1193(17) -0.0274(14) -0.0180(13) -0.0397(14) C19 0.0650(14) 0.0576(13) 0.0609(13) -0.0005(11) 0.0105(11) -0.0191(11) C9 0.0606(14) 0.0675(15) 0.0669(14) 0.0084(12) -0.0075(11) 0.0223(12) C5 0.0690(15) 0.0547(13) 0.0681(14) -0.0004(11) 0.0015(11) 0.0029(12) C18 0.0601(14) 0.0630(14) 0.0690(14) 0.0163(11) 0.0096(11) -0.0083(12) C8 0.0474(12) 0.0747(15) 0.0735(14) 0.0156(12) 0.0007(11) 0.0109(13) C2 0.0615(14) 0.100(2) 0.0540(13) 0.0235(14) -0.0013(10) 0.0112(14) C1 0.0797(18) 0.086(2) 0.0766(17) 0.0393(16) 0.0147(14) 0.0276(16) C6 0.095(2) 0.0514(14) 0.0954(19) 0.0169(14) 0.0168(16) 0.0094(14) O4B 0.081(5) 0.040(3) 0.106(6) 0.015(3) -0.021(4) -0.014(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 C20 N2 C14 . . 124.81(15) ? C17 N2 C14 . . 125.19(15) ? C17 N2 C20 . . 109.84(16) ? C7 N1 C4 . . 123.81(16) ? C10 N1 C4 . . 125.65(16) ? C10 N1 C7 . . 109.61(16) ? O8 N4 O7 . . 124.03(18) ? O8 N4 C13 . . 118.58(16) ? O7 N4 C13 . . 117.37(18) ? C14 C13 N4 . . 121.04(16) ? C12 C13 N4 . . 117.50(16) ? C12 C13 C14 . . 121.45(17) ? C13 C14 N2 . . 122.56(16) ? C15 C14 N2 . . 119.17(16) ? C15 C14 C13 . . 118.24(17) ? O4A N3 C3 . . 116.5(7) ? O3 N3 O4A . . 125.8(7) ? O3 N3 C3 . . 117.4(2) ? O4B N3 C3 . . 121.0(4) ? O4B N3 O3 . . 121.4(5) ? C3 C4 N1 . . 122.75(18) ? C5 C4 N1 . . 119.45(18) ? C5 C4 C3 . . 117.80(19) ? C13 C12 H12 . . 120.2 ? C11 C12 C13 . . 119.52(18) ? C11 C12 H12 . . 120.2 ? C14 C15 H15 . . 120.0 ? C16 C15 C14 . . 120.04(19) ? C16 C15 H15 . . 120.0 ? N2 C20 C19 . . 106.06(17) ? O6 C20 N2 . . 124.78(19) ? O6 C20 C19 . . 129.16(19) ? N2 C17 C18 . . 105.62(17) ? O5 C17 N2 . . 125.12(19) ? O5 C17 C18 . . 129.25(19) ? C4 C3 N3 . . 120.01(19) ? C2 C3 N3 . . 118.0(2) ? C2 C3 C4 . . 122.0(2) ? N1 C7 C8 . . 106.01(18) ? O2 C7 N1 . . 124.43(19) ? O2 C7 C8 . . 129.5(2) ? C12 C11 H11 . . 120.2 ? C12 C11 C16 . . 119.69(19) ? C16 C11 H11 . . 120.2 ? C15 C16 C11 . . 121.02(19) ? C15 C16 H16 . . 119.5 ? C11 C16 H16 . . 119.5 ? N1 C10 C9 . . 105.79(18) ? O1 C10 N1 . . 124.88(19) ? O1 C10 C9 . . 129.3(2) ? C20 C19 H19 . . 125.5 ? C18 C19 C20 . . 109.02(19) ? C18 C19 H19 . . 125.5 ? C10 C9 H9 . . 125.4 ? C8 C9 C10 . . 109.3(2) ? C8 C9 H9 . . 125.4 ? C4 C5 H5 . . 119.7 ? C6 C5 C4 . . 120.6(2) ? C6 C5 H5 . . 119.7 ? C17 C18 H18 . . 125.3 ? C19 C18 C17 . . 109.39(19) ? C19 C18 H18 . . 125.3 ? C7 C8 H8 . . 125.5 ? C9 C8 C7 . . 108.97(19) ? C9 C8 H8 . . 125.5 ? C3 C2 H2 . . 120.7 ? C1 C2 C3 . . 118.6(2) ? C1 C2 H2 . . 120.7 ? C2 C1 H1 . . 119.7 ? C6 C1 C2 . . 120.6(2) ? C6 C1 H1 . . 119.7 ? C5 C6 H6 . . 119.8 ? C1 C6 C5 . . 120.4(2) ? C1 C6 H6 . . 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 N2 C14 . 1.419(2) ? N2 C20 . 1.394(2) ? N2 C17 . 1.393(2) ? O6 C20 . 1.205(2) ? O8 N4 . 1.215(2) ? N1 C4 . 1.416(2) ? N1 C7 . 1.389(2) ? N1 C10 . 1.388(3) ? O5 C17 . 1.200(2) ? N4 O7 . 1.222(2) ? N4 C13 . 1.460(2) ? O2 C7 . 1.207(2) ? O1 C10 . 1.200(2) ? C13 C14 . 1.391(2) ? C13 C12 . 1.377(3) ? C14 C15 . 1.382(3) ? N3 O4A . 1.261(15) ? N3 C3 . 1.465(3) ? N3 O3 . 1.230(3) ? N3 O4B . 1.164(11) ? C4 C3 . 1.381(3) ? C4 C5 . 1.381(3) ? C12 H12 . 0.9300 ? C12 C11 . 1.369(3) ? C15 H15 . 0.9300 ? C15 C16 . 1.375(3) ? C20 C19 . 1.475(3) ? C17 C18 . 1.481(3) ? C3 C2 . 1.377(3) ? C7 C8 . 1.473(3) ? C11 H11 . 0.9300 ? C11 C16 . 1.377(3) ? C16 H16 . 0.9300 ? C10 C9 . 1.475(3) ? C19 H19 . 0.9300 ? C19 C18 . 1.308(3) ? C9 H9 . 0.9300 ? C9 C8 . 1.304(3) ? C5 H5 . 0.9300 ? C5 C6 . 1.373(3) ? C18 H18 . 0.9300 ? C8 H8 . 0.9300 ? C2 H2 . 0.9300 ? C2 C1 . 1.372(4) ? C1 H1 . 0.9300 ? C1 C6 . 1.362(4) ? C6 H6 . 0.9300 ? 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 C5 H5 O7 2_545 0.93 2.636 3.457(3) 147.56 C18 H18 O5 2_645 0.93 2.611 3.343(3) 135.92 C16 H16 O3 3_676 0.93 2.785 3.210(3) 108.94 C15 H15 O5 2_655 0.93 2.675 3.455(3) 141.89 C19 H19 O2 4_665 0.93 2.606 3.362(3) 138.81 C19 H19 O6 3_665 0.93 2.612 3.388(3) 141.33 C2 H2 O1 3_666 0.93 2.655 3.358(3) 132.94 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N2 C14 C15 C16 . . . . 179.26(18) ? N2 C20 C19 C18 . . . . 1.9(3) ? N2 C17 C18 C19 . . . . -1.3(3) ? O6 C20 C19 C18 . . . . -177.2(2) ? O8 N4 C13 C14 . . . . 38.8(2) ? O8 N4 C13 C12 . . . . -139.90(19) ? N1 C4 C3 N3 . . . . 0.9(3) ? N1 C4 C3 C2 . . . . -179.20(19) ? N1 C4 C5 C6 . . . . -179.2(2) ? N1 C7 C8 C9 . . . . -3.9(3) ? N1 C10 C9 C8 . . . . 3.0(3) ? O5 C17 C18 C19 . . . . 177.4(3) ? N4 C13 C14 N2 . . . . 3.9(3) ? N4 C13 C14 C15 . . . . -178.18(16) ? N4 C13 C12 C11 . . . . 176.92(17) ? O2 C7 C8 C9 . . . . 174.7(2) ? O7 N4 C13 C14 . . . . -142.47(18) ? O7 N4 C13 C12 . . . . 38.8(2) ? O1 C10 C9 C8 . . . . -174.7(3) ? C13 C14 C15 C16 . . . . 1.3(3) ? C13 C12 C11 C16 . . . . 1.3(3) ? C14 N2 C20 O6 . . . . 0.9(3) ? C14 N2 C20 C19 . . . . -178.29(17) ? C14 N2 C17 O5 . . . . -0.7(3) ? C14 N2 C17 C18 . . . . 178.04(18) ? C14 C13 C12 C11 . . . . -1.8(3) ? C14 C15 C16 C11 . . . . -1.7(3) ? N3 C3 C2 C1 . . . . 177.8(2) ? O4A N3 C3 C4 . . . . 43.2(9) ? O4A N3 C3 C2 . . . . -136.7(9) ? C4 N1 C7 O2 . . . . -3.3(3) ? C4 N1 C7 C8 . . . . 175.37(18) ? C4 N1 C10 O1 . . . . 3.1(4) ? C4 N1 C10 C9 . . . . -174.82(18) ? C4 C3 C2 C1 . . . . -2.1(3) ? C4 C5 C6 C1 . . . . -1.1(4) ? C12 C13 C14 N2 . . . . -177.44(17) ? C12 C13 C14 C15 . . . . 0.5(3) ? C12 C11 C16 C15 . . . . 0.4(3) ? C20 N2 C14 C13 . . . . 51.8(3) ? C20 N2 C14 C15 . . . . -126.1(2) ? C20 N2 C17 O5 . . . . -176.2(2) ? C20 N2 C17 C18 . . . . 2.5(2) ? C20 C19 C18 C17 . . . . -0.4(3) ? C17 N2 C14 C13 . . . . -123.1(2) ? C17 N2 C14 C15 . . . . 59.0(3) ? C17 N2 C20 O6 . . . . 176.4(2) ? C17 N2 C20 C19 . . . . -2.8(2) ? C3 C4 C5 C6 . . . . 1.3(3) ? C3 C2 C1 C6 . . . . 2.4(4) ? C7 N1 C4 C3 . . . . -100.0(2) ? C7 N1 C4 C5 . . . . 80.6(3) ? C7 N1 C10 O1 . . . . 172.4(2) ? C7 N1 C10 C9 . . . . -5.5(2) ? C10 N1 C4 C3 . . . . 67.8(3) ? C10 N1 C4 C5 . . . . -111.6(2) ? C10 N1 C7 O2 . . . . -172.8(2) ? C10 N1 C7 C8 . . . . 5.9(2) ? C10 C9 C8 C7 . . . . 0.5(3) ? O3 N3 C3 C4 . . . . -142.3(2) ? O3 N3 C3 C2 . . . . 37.8(3) ? C5 C4 C3 N3 . . . . -179.7(2) ? C5 C4 C3 C2 . . . . 0.2(3) ? C2 C1 C6 C5 . . . . -0.9(4) ? O4B N3 C3 C4 . . . . 32.9(8) ? O4B N3 C3 C2 . . . . -147.0(8) ? _cod_database_fobs_code 2023023